تفاعل #614780

معادلة التفاعل

1,1-dimethylethyl[1,1-dimethyl-2-({6-[(1a-methyl-1,1a,2,7b-tetrahydrocyclopropa[c]chromen-7-yl)oxy]-3-pyridinyl}amino)-2-oxoethyl]carbamate

Intermediate 128

1,1-dimethylethyl[1,1-dimethyl-2-({6-[(1a-methyl-1,1a,2,7b-tetrahydrocyclopropa[c]chromen-7-yl)oxy]-3-pyridinyl}amino)-2-oxoethyl]carbamate

TFA

→

title compound

2-methyl-N1-{6-[(1a-methyl-1,1a,2,7b-tetrahydrocyclopropa[c]chromen-7-yl)oxy]-3-pyridinyl}alaninamide

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىat 0° C
2. 2
   أخرىThe solvent and the excess of TFA were evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane
4. 4
   workup.ADDITIONa saturated solution of NaHCO3 was slowly added while the pH
5. 5
   أخرىTwo phases were separated
6. 6
   تجفيفthe organic layer was dried over sodium sulphate
7. 7
   ترشيحfiltered
8. 8
   أخرىevaporated

الإجراء التجريبي

To a solution of 1,1-dimethylethyl[1,1-dimethyl-2-({6-[(1a-methyl-1,1a,2,7b-tetrahydrocyclopropa[c]chromen-7-yl)oxy]-3-pyridinyl}amino)-2-oxoethyl]carbamate (Intermediate 128, 135 mg, 0.298 mmol) in dry dichloromethane (10 ml) at 0° C. TFA (5 ml, 64.9 mmol) was slowly added and the reaction mixture was stirred for 2 hours at the same temperature. The solvent and the excess of TFA were evaporated and the residue was dissolved in dichloromethane and a saturated solution of NaHCO3 was slowly added while the pH was allowed to reach 8. Two phases were separated and the organic layer was dried over sodium sulphate, filtered and evaporated affording the title compound as a colourless oil used as it was without any further purification (105 mg).

المصدر