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

N,N-Dimethylaniline → 16beta-Ethyl-17beta-(2-methylvaleryl)oxyacetoxy-4-estren-3-one

HRID 64724
ノート
印刷プレビュー

反応式

HRID 64724 の反応式
[CH2:1]([C@H:3]1[CH2:8][C@H:7]2[C@H:9]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C@H:4]1[O:22][C:23](=[O:26])[CH2:24][OH:25])[C@@H:17]1[C:12](=[CH:13][C:14](=[O:21])[CH2:15][CH2:16]1)[CH2:11][CH2:10]3)[CH3:2].CN(C)C1C=CC=CC=1.[CH3:36][CH:37]([CH2:41][CH2:42][CH3:43])[C:38](Cl)=[O:39]>ClCCl.C(OCC)(=O)C>[CH2:1]([C@H:3]1[CH2:8][C@H:7]2[C@H:9]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C@H:4]1[O:22][C:23](=[O:26])[CH2:24][O:25][C:38](=[O:39])[CH:37]([CH3:36])[CH2:41][CH2:42][CH3:43])[C@@H:17]1[C:12](=[CH:13][C:14](=[O:21])[CH2:15][CH2:16]1)[CH2:11][CH2:10]3)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 949N,N-DimethylanilineHCID 1073852-Methylvaleryl chlorideHCID 7046644116beta-Ethyl-17beta-glycoloyloxy-4-estren-3-one

生成物 1

HCID 7046693016beta-Ethyl-17beta-(2-methylvaleryl)oxyacetoxy-4-estren-3-one収率 19.8%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

In 20 ml of dichloromethane are dissolved 0.5 g of 16β-ethyl-17β-glycoloyloxy-4-estren-3-one and 0.2 ml of N,N-dimethylaniline, and 0.5 g of 2-methylvaleryl chloride is added to the above solution. The mixture is refluxed for 6 hours. After cooling, the reaction mixture is diluted with 150 ml of ethyl acetate and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 200 ml of diisopropyl ether-n-hexane (2:8), elution is carried out with 500 ml of a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.126 g of the above-identified compound as a light-yellow viscous oil.

後処理

  1. additionis added to the above solution
  2. temperatureThe mixture is refluxed for 6 hours
  3. temperatureAfter cooling
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent is then distilled off under reduced pressure
  6. washpassage of 200 ml of diisopropyl ether-n-hexane (2:8), elution
  7. additionis carried out with 500 ml of a 1:1 mixture of the same solvents
  8. customThe eluate is evaporated under reduced pressure
  9. customto remove the solvent

出典と根拠

ORDレコード
ord-6c373de8ad0a482ca08749a90e9f07a1
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04609650

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