1,1-Dimethylhydrazine → beta-Carboline-3-carboxaldehyde-dimethylhydrazone

HRID 1982447노트

반응식

HRID 1982447 반응식
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[C:3]([CH:14]=O)[N:2]=1.CN(C)C=O.[CH3:21][N:22]([CH3:24])[NH2:23]>O>[CH3:21][N:22]([CH3:24])[N:23]=[CH:14][C:3]1[N:2]=[CH:1][C:13]2[NH:12][C:11]3[C:6]([C:5]=2[CH:4]=1)=[CH:7][CH:8]=[CH:9][CH:10]=3

참가 물질

5

반응물 3

HCID 59761,1-DimethylhydrazineHCID 6228DimethylformamideHCID 127891449H-pyrido[3,4-b]indole-3-carbaldehyde

생성물 1

HCID 54038756beta-Carboline-3-carboxaldehyde-dimethylhydrazone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.0 g of beta-carboline-3-carboxaldehyde, 10 ml of dimethyl-formamide and 3 ml of N,N-dimethyl hydrazine is introduced into a glass autoclave. The air is replaced by nitrogen. After stirring for 3 h, the reaction mixture is allowed to stand overnight at room temperature. After adding 25 ml of water, the reaction mixture is extracted with 100 and 50 ml of chloroform. The chloroform phase is dried using magnesium sulfate, then filtered. Then, the chloroform is evaporated. After adding 10 ml of ether, the reaction product is filtered off. 0.9 g of beta-carboline-3-carboxaldehyde-dimethylhydrazone with a m.p. of 203°-206° C. is obtained.

후처리

  1. additionis introduced into a glass autoclave
  2. waitto stand overnight at room temperature
  3. extractionthe reaction mixture is extracted with 100 and 50 ml of chloroform
  4. dry with materialThe chloroform phase is dried
  5. filtrationfiltered
  6. customThen, the chloroform is evaporated
  7. additionAfter adding 10 ml of ether
  8. filtrationthe reaction product is filtered off

출처 및 근거

ORD 기록
ord-e7767aecb0404b3a8328b02e3b7c5155
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04596808

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