تفاعل #66853

معادلة التفاعل

solution

7-[(2E)-4-Chlorobut-2-enoyl]-N-(3,4-dichlorophenyl)-5,6,7,8-tetrahydropyrido[4′,3′:4,5]thieno[2,3-d]pyrimidin-4-amine

DIPEA

1,4-oxazepane hydrochloride

→

title compound

المردود 80.0%

N-(3,4-Dichlorophenyl)-7-[(2E)-4-(1,4-oxazepan-4-yl)but-2-enoyl]-5,6,7,8-tetrahydropyrido[4′,3′:4,5]thieno[2,3-d]pyrimidin-4-amine

المردود 80.0%

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated for 1 h to 50° C
2. 2
   أخرىThe reaction mixture was directly separated by preparative HPLC
3. 3
   أخرىThe product crystallized upon trituration with dichloromethane
4. 4
   أخرىThe solvent was removed in vacuo

الإجراء التجريبي

To a solution of Example 59A (100 mg, 0.201 mmol) in DMF (2 mL) and DIPEA (0.10 mL, 0.60 mmol) was added 1,4-oxazepane hydrochloride (55 mg, 0.40 mmol). The mixture was stirred for 1 h at rt and then heated for 1 h to 50° C. The reaction mixture was directly separated by preparative HPLC. The product crystallized upon trituration with dichloromethane. The solvent was removed in vacuo to yield 83 mg (80%) of the title compound.

المصدر