Toluene → HCID 178483213、化合物

HRID 485384ノート

反応式

HRID 485384 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

HCID 178483213HCID 178483213、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-792de627416c41c5b13218234da18c6c
出典データセット
uspto-grants-1985_08
特許番号
US04536508

反応ノート

読み込み中…