Triethylene Glycol → 2-(4-Chlorobenzyl)-1-[4-(4-fluorophenyl)butyl]perhydroazepine

HRID 27435

반응식

HRID 27435 반응식
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][CH:7]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][N:8]2[CH2:14][CH2:15][CH2:16][C:17](=O)[C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[CH:4][CH:3]=1.O.NN.[OH-].[K+].C(O)COCCOCCO>C(OCC)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH:7]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][N:8]2[CH2:14][CH2:15][CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([F:24])=[CH:22][CH:23]=2)=[CH:26][CH:27]=1

참가 물질

7

반응물 4

HCID 8172Triethylene GlycolHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 233428532-(4-Chlorobenzyl)-1-[3-(4-fluorobenzoyl)propyl]perhydroazepine

생성물 1

HCID 233428342-(4-Chlorobenzyl)-1-[4-(4-fluorophenyl)butyl]perhydroazepine수율 62.2%

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

Heat 0.5 g of the title compound of Example 39 with 1 ml of hydrazine hydrate, 0.5 g of potassium hydroxide and 5 ml of triglycol for 2 hours at 165°. Cool the resulting reaction mixture to ambient temperature. Mix the cooled reaction mixture with water and diethyl ether. Dry the ether phase over sodium sulfate and then concentrate it to obtain 0.3 g of the title compound as a viscous oil.

후처리

  1. temperatureCool
  2. customthe resulting reaction mixture to ambient temperature
  3. additionMix
  4. dry with materialDry the ether phase over sodium sulfate
  5. concentrationconcentrate it

출처 및 근거

ORD 기록
ord-263ae71c66374e658004a1b702d7a9d6
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221788

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