Water → 2-Benzyloxy-7,8,9,10-tetrahydro-11-phenyl-6H-azepino[1,2-a]indole

HRID 66828ノート

反応式

HRID 66828 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[N:14]1[CH2:18][CH2:19][CH2:20][CH2:21][C:22](=O)[C:13]1=[C:12]2[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN.[OH-].[K+].O>C(O)COCCOCCO>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[N:14]1[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:13]1=[C:12]2[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 20529096HCID 20529096、化合物

生成物 1

HCID 205291872-Benzyloxy-7,8,9,10-tetrahydro-11-phenyl-6H-azepino[1,2-a]indole

試薬・触媒・溶媒 1

HCID 8172Triethylene Glycol溶媒

実験手順

An amount of 2.3 g (6 m mole) of 2-benzyloxy-7,8,9,10-tetrahydro-10-oxo-11-phenyl-6H-azepino[1,2-a]indole 4.5 ml of 80% hydrazine hydrate and 1.5 g of potassium hydroxide were heated in 6 ml of triethylene-glycol for two hours to 180° C. and for four hours to 220° C. After cooling, the reaction mixture was mixed with water and extracted with chloroform. After evaporation of the chloroform extracts, the residue was purified by column chromatography on silicagel (solvent: toluene). When the eluates were evaporated, colorless crystals were obtained.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with chloroform
  3. customAfter evaporation of the chloroform
  4. customthe residue was purified by column chromatography on silicagel (solvent: toluene)
  5. customWhen the eluates were evaporated
  6. customcolorless crystals were obtained

出典と根拠

ORDレコード
ord-54c84805a4a74fbbbbfc6dae3c3b6578
出典データセット
uspto-grants-1982_08
特許番号
US04343811

反応ノート

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