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

HRID 66828노트

반응식

HRID 66828 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 20529096HCID 20529096, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8172Triethylene Glycol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-54c84805a4a74fbbbbfc6dae3c3b6578
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343811

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