ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → Ethyl 7-{[4-(acetyloxy)nonyl](cyano)amino}heptanoate

HRID 1729911
ノート
印刷プレビュー

反応式

HRID 1729911 の反応式
[H-].[Na+].[NH:3]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]#[N:5].Cl[CH2:18][CH2:19][CH2:20][CH:21]([O:27][C:28](=[O:30])[CH3:29])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].O>C1C=CC=CC=1.CN(C)C=O>[C:28]([O:27][CH:21]([CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[CH2:20][CH2:19][CH2:18][N:3]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]#[N:5])(=[O:30])[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 131047161-Chloro-4-acetoxynonaneHCID 21501476Ethyl 7-(cyanoamino)heptanoate

生成物 1

HCID 71444712Ethyl 7-{[4-(acetyloxy)nonyl](cyano)amino}heptanoate

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回
HCID 6228
Dimethylformamide
溶媒

実験手順

Sodium hydride (57%, in mineral oil) (0.48 g., 0.01 mole) is washed twice with benzene then suspended in benzene (50 ml.) and dimethylformamide (50 ml.). Ethyl 7-cyanamidoheptanoate (1.98 g. 0.01 mole) (Example N, Step 2) is added and the suspension heated on the steam bath for 15 minutes. The reaction mixture is cooled to room temperature, 1-chloro-4-acetoxynonane (2.6 g., 0.01 mole) (Example A, Step 3) is added and then the reaction is heated on the steam bath for 2 hours then stirred 18 hours at room temperature. The reaction is poured into water (300 ml.) and extracted with benzene (3 × 100 ml.). The benzene is washed with brine then dried over sodium sulfate. Removal of the solvent yields an oil which is purified by silica gel chromatography, elution solvent 3% methanol in chloroform, evaporation of the appropriate fraction affords ethyl 7-[N-(4-acetoxynonyl) cyanamido]-heptanoate. The yield is 3.2 g. (83 %).

後処理

  1. temperaturethe suspension heated on the steam bath for 15 minutes
  2. temperaturethe reaction is heated on the steam bath for 2 hours
  3. extractionextracted with benzene (3 × 100 ml.)
  4. washThe benzene is washed with brine
  5. dry with materialthen dried over sodium sulfate
  6. customRemoval of the solvent
  7. customyields an oil which
  8. customis purified by silica gel chromatography, elution solvent 3% methanol in chloroform, evaporation of the appropriate fraction

出典と根拠

ORDレコード
ord-7f39267595ec464295f68f56c928d005
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03989749

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート