Dimethylformamide → HCID 563927, 화합물

HRID 68546노트

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HRID 68546 반응식
[C:1]1([N:7]2[C:12](=[O:13])[NH:11][C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CN(C=O)C.[H-].[Na+].[CH2:24](Br)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>O>[C:1]1([N:7]2[C:12](=[O:13])[N:11]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:10](=[O:14])[C:9]([C:15]#[N:16])=[N:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 563387HCID 563387, 화합물

생성물 1

HCID 563927HCID 563927, 화합물수율 81%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Intermediate c (9 g, 0.042 mol) was added to DMF (80 mL) under an ice bath. To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, benzyl bromide (3.1 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted at 50° C. for 4 h. After completion of the reaction, the reaction solution was poured into water (300 mL). A great deal of solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce Intermediate j (8.1 g) in a yield of 81%.

후처리

  1. additionAfter the dropwise addition
  2. waitthe reaction was conducted at 50° C. for 4 h
  3. customAfter completion of the reaction
  4. customA great deal of solid separated out
  5. filtrationwas filtered by suction
  6. washThe filtered cake was washed with water
  7. customdried

출처 및 근거

ORD 기록
ord-f0f5808a8e87425f93585dd81c4da0ed
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822465B2

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