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

HRID 27435

反応式

HRID 27435 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-263ae71c66374e658004a1b702d7a9d6
出典データセット
uspto-grants-1980_09
特許番号
US04221788

関連ノート

読み込み中…