반응 #1340051

반응 방정식

2,2-dimethyl-1,3-benzodithiole-4-sulfonamide

2,2-Dimethyl-1,3-Benzodithiole-4-Sulfonamide

trimethylaluminum

acetic acid

methyl [4-methoxy-6-methyl-1,3,5-triazin-2-yl]carbamate

→

N-[(4-Methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2,2-dimethyl-1,3-benzodithiole-4-sulfonamide

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도the reaction mixture was heated
3. 3
   온도at reflux for 72 hours
4. 4
   온도The reaction mixture was cooled to room temperature
5. 5
   기타The organic phase was separated
6. 6
   기타dried
7. 7
   기타the solvent removed under reduced pressure
8. 8
   기타to give an oil
9. 9
   기타Crystallization of the oil from an appropriate solvent
10. 10
    기타gave a solid

실험 절차

To a solution of 2.6 g 2,2-dimethyl-1,3-benzodithiole-4-sulfonamide prepared in Example 7, in 60 ml methylene chloride at room temperature under nitrogen is added 5.5 ml trimethylaluminum (2M in toluene). After stirring 15 minutes at room temperature, 2.0 g of methyl [4-methoxy-6-methyl-1,3,5-triazin-2-yl]carbamate, prepared according to the procedure of Example 5, was added and the reaction mixture was heated at reflux for 72 hours. The reaction mixture was cooled to room temperature and 75 ml ice, 3 ml glacial acetic acid, and 10 drops of hydrochloric acid were sequentially added. The organic phase was separated, dried and the solvent removed under reduced pressure to give an oil. Crystallization of the oil from an appropriate solvent gave a solid.

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