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

tert-Butanol → tert-Butyl 2-(4-tert-butyldimethylsilyloxymethyl-2-propylphenoxy)-2-phenylacetate

HRID 1492631
ノート
印刷プレビュー

反応式

HRID 1492631 の反応式
[Si:1]([O:8][CH2:9][C:10]1[CH:26]=[CH:25][C:13]([O:14][CH:15]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:16]([OH:18])=[O:17])=[C:12]([CH2:27][CH2:28][CH3:29])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(Cl)(=O)C(Cl)=O.[C:36](O)([CH3:39])([CH3:38])[CH3:37].CCN(CC)CC>C1C=CC=CC=1.CN(C=O)C.C(Cl)Cl.CCOC(C)=O>[Si:1]([O:8][CH2:9][C:10]1[CH:26]=[CH:25][C:13]([O:14][CH:15]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:16]([O:18][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:17])=[C:12]([CH2:27][CH2:28][CH3:29])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 6386tert-ButanolHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 193855972-(4-Tert-butyldimethylsilyloxymethyl-2-propylphenoxy)-2-phenylacetic acid

生成物 1

HCID 19385645tert-Butyl 2-(4-tert-butyldimethylsilyloxymethyl-2-propylphenoxy)-2-phenylacetate収率 73.8%

試薬・触媒・溶媒 4

HCID 6228
Dimethylformamide
触媒
HCID 241Benzene溶媒
HCID 6344Dichloromethane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 929 mg (2.24 mmol) of the product of Step L in benzene were added oxalyl chloride (234 mL, 2.69 mmol) and one drop of DMF at 0° C. The solution was stirred at rt for 45 minutes. After concentration the residue was dissolved in CH2Cl2 (10 mL). The solution was added to a solution of tert-butyl alcohol (253 mL, 2.69 mmol) and Et3N in CH2Cl2 (10 mL) at 0° C. The solution was stirred at rt for 3 hours. The mixture was poured into EtOAc (50 mL) and washed with H2O (1×) and brine, and dried over anhydrous MgSO4. Concentration gave 778 mg of the title compound as a slightly yellow glass.

後処理

  1. concentrationAfter concentration the residue
  2. dissolutionwas dissolved in CH2Cl2 (10 mL)
  3. stirringThe solution was stirred at rt for 3 hours
  4. washwashed with H2O (1×) and brine
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationConcentration

出典と根拠

ORDレコード
ord-1ae1db06131846958118729ef8e22cf7
出典データセット
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05374638

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