Chloroacetyl chloride → 4-(2-chloroacetyl)-3,5-dimethyl-1H-pyrrole-2-carbaldehyde
반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][C:6]1[CH:10]=[C:9]([CH3:11])[NH:8][C:7]=1[CH:12]=[O:13].[Cl:14][CH2:15][C:16](Cl)=[O:17]>ClCCCl>[Cl:14][CH2:15][C:16]([C:10]1[C:6]([CH3:5])=[C:7]([CH:12]=[O:13])[NH:8][C:9]=1[CH3:11])=[O:17]참가 물질
5
실험 절차
Anhydrous aluminum chloride (42 g, 315 mmol) was added portionwise over 30 min to a room temperature solution of 3,5-dimethylpyrrol-2-carboxaldehyde (5 g, 40 mmol) in 1,2-dichloroethane (50 ml) under nitrogen. After stirring for 15 min, chloroacetyl chloride (17 g, 150 mmol) was added dropwise over 1 h. After addition was complete, the mixture was stirred at room temperature for 16 h. The mixture was poured onto crushed ice and the organic layer separated, dried over anhydrous sodium sulfate, and the solvent removed under reduced pressure. Yield 57%, m.p. 205–09° C. (toluene).
후처리
- additionAfter addition
- stirringthe mixture was stirred at room temperature for 16 h
- additionThe mixture was poured
- customonto crushed ice
- customthe organic layer separated
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent removed under reduced pressure
출처 및 근거
- ORD 기록
- ord-e226a92232d04cdc97ffba1e1b7b32aa
- 출처 데이터셋
- uspto-grants-2006_06
- 특허 번호
- US07060822B1
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