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

Ammonium Chloride → 1-({[tert-Butyl(diphenyl)silyl]oxy}methyl)cyclopropan-1-ol

HRID 1820610
ノート
印刷プレビュー

反応式

HRID 1820610 の反応式
[Si:1]([O:18][CH2:19][C:20]([O:22]CC)=O)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:25]([Mg]Br)[CH3:26].[Cl-].[NH4+]>O1CCCC1.CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[Si:1]([O:18][CH2:19][C:20]1([OH:22])[CH2:26][CH2:25]1)([C:14]([CH3:15])([CH3:17])[CH3:16])([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 25517Ammonium ChlorideHCID 59464758(tert-Butyl-diphenyl-silanyloxy)-acetic acid ethyl esterHCID 178418443HCID 178418443、化合物

生成物 1

HCID 529878051-({[tert-Butyl(diphenyl)silyl]oxy}methyl)cyclopropan-1-ol収率 100%

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

According to the description in a reference (see: Syn. Lett. 07, 1053-1054, 1999), the title compound was prepared as follows. 12 g (35 mmole) of ethyl 2-{[t-butyl(diphenyl)silyl]oxy}acetate was dissolved in 200 ml of tetrahydrofuran (THF) and 2.2 ml of titaniumtetraisopropoxide was added thereto. To the mixture was slowly added 29.2 ml of ethylmagnesiumbromide (3.0M in THF), and the reaction solution was stirred for 12 hours at room temperature. 20 ml of saturated ammonium chloride was added to stop the reaction. About 150 ml of tetrahydrofuran (THF) used as a solvent was removed by distillation under reduced pressure, and the reaction mixture was extracted twice with 200 ml of ethyl acetate. The ethyl acetate extract was distilled under reduced pressure to give 11.4 g (Yield 100%) of the title compound as a white solid.

後処理

  1. customthe title compound was prepared
  2. customthe reaction
  3. customwas removed by distillation under reduced pressure
  4. extractionthe reaction mixture was extracted twice with 200 ml of ethyl acetate
  5. extractionThe ethyl acetate extract
  6. distillationwas distilled under reduced pressure

出典と根拠

ORDレコード
ord-45e0c26fb45541f0b3e3c1bbed432384
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07605147B2

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