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

Dimethyl Sulfoxide → (R)-1-[3-(tertbutyldiphenyl-silyloxy)benzyl]-1-trimethylsilyoxy-2-cyclohexanone

HRID 379313
ノート
印刷プレビュー

反応式

HRID 379313 の反応式
C(Cl)(C(Cl)=O)=O.CS(C)=O.[C:11]([Si:15]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[O:16][C:17]1[CH:18]=[C:19]([CH:29]=[CH:30][CH:31]=1)[CH2:20][C@:21]1([OH:28])[CH2:26][CH2:25][CH2:24][CH2:23][C@H:22]1[OH:27])([CH3:14])([CH3:13])[CH3:12].N1C=CN=C1>C(Cl)Cl.CN(C=O)C.C(N(CC)CC)C>[C:11]([Si:15]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)[O:16][C:17]1[CH:18]=[C:19]([CH:29]=[CH:30][CH:31]=1)[CH2:20][C@:21]1([O:28][Si:15]([CH3:38])([CH3:32])[CH3:11])[CH2:26][CH2:25][CH2:24][CH2:23][C:22]1=[O:27])([CH3:14])([CH3:12])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 679Dimethyl SulfoxideHCID 795ImidazoleHCID 65578Oxalyl chlorideHCID 20691700(1R,2R)-1-[3-(tertbutyldiphenylsilyloxy)benzyl]-1,2-dihydroxycyclohexane

生成物 1

HCID 86757468(R)-1-[3-(tertbutyldiphenyl-silyloxy)benzyl]-1-trimethylsilyoxy-2-cyclohexanone収率 16.6%

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒2 回
HCID 8471Triethylamine溶媒

実験手順

To a solution of (COCl)2 (3.4 ml) in CH2Cl2 (100 ml) was dropwise added DMSO (3.7 ml) at −78° C. After 10minutes, a solution of (1R,2R)-1-[3-(tertbutyldiphenylsilyloxy)benzyl]-1,2-dihydroxycyclohexane (12 g) in CH2Cl2(50 ml) was added to the above mixture at the same temperature. After 10 minutes, the mixture was added with triethylamine (15 ml) and allowed to stand at room temperature. After evaporating the solvent, the residue was partitioned between EtOAc and water. The organic layer was washed with water and brine. The organic solvent was evaporated in vacuo to give an oily compound. The oily compound was dissolved in DMF (50 ml) and then added with trimethylsilychloride (6.6 ml) and imidazole(7.0 g) at room temperature. After stirring for 5 hours, the mixture was partitioned between EtOAc and water. The organic solvent was evaporated in vacuo. The residue was purified by chromatography on silica gel to give (R)-1-[3-(tertbutyldiphenylsilyloxy)benzyl]-1-trimethylsilyoxy-2-cyclohexanone (1.15 g).

後処理

  1. customat −78° C
  2. waitAfter 10 minutes
  3. customto stand at room temperature
  4. customAfter evaporating the solvent
  5. customthe residue was partitioned between EtOAc and water
  6. washThe organic layer was washed with water and brine
  7. customThe organic solvent was evaporated in vacuo
  8. customto give an oily compound
  9. customthe mixture was partitioned between EtOAc and water
  10. customThe organic solvent was evaporated in vacuo
  11. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-91f65fd9404d4da1938e65b402e775b5
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06297267B1

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