Toluene → HCID 178483213, 화합물

HRID 485384노트

반응식

HRID 485384 반응식
[CH3:1][N:2]([CH2:4][C:5]1[CH:6]=[C:7]([CH:14]=[CH:15][CH:16]=1)[O:8][CH2:9][CH2:10][CH2:11][CH:12]=O)[CH3:3].[C:17]1([C:23]2[N:27]=[C:26]([NH2:28])[N:25](C)[N:24]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[C:30]1(C)C=CC=CC=1>>[CH3:1][N:2]([CH2:4][C:5]1[CH:6]=[C:7]([CH:14]=[CH:15][CH:16]=1)[O:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:28][C:26]1[NH:25][N:24]=[C:23]([CH2:17][C:22]2[CH:30]=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:27]=1)[CH3:3]

참가 물질

4

반응물 3

HCID 1140TolueneHCID 125813071-methyl-3-phenyl-1H-1,2,4-triazol-5-amineHCID 20270275HCID 20270275, 화합물

생성물 1

HCID 178483213HCID 178483213, 화합물

실험 절차

A solution of 4-[3-[(dimethylamino)methyl]phenoxy]butanal (0.5 g) and 3-phenyl methyl-1H-1,2,4-triazole-5-amine (0.39 g) in dry toluene (60 ml) was heated under reflux during 3 h. The solvent was evaporated and replaced with methanol (50 ml). Sodium borohydride (0.4 g) was added and the mixture was stirred at 20° during 2 h. The methanol was evaporated and the residue partitioned between water and ethyl acetate. The organic extract was evaporated and the residue was purified by column chromatography to give the title compound, which crystallised from a mixture of ethyl acetate and cyclohexane as pale yellow crystals (0.09 g) m.p. 131°-3°; tlc system A,Rf 0.6.

후처리

  1. temperatureunder reflux during 3 h
  2. customThe solvent was evaporated
  3. additionSodium borohydride (0.4 g) was added
  4. customThe methanol was evaporated
  5. customthe residue partitioned between water and ethyl acetate
  6. extractionThe organic extract
  7. customwas evaporated
  8. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-792de627416c41c5b13218234da18c6c
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536508

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