Isopropanol → Ethyl isopropoxyacetate

HRID 18809

反応式

HRID 18809 の反応式
[CH3:1][CH:2]([OH:4])[CH3:3].[N+](=[CH:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[N-]>ClCCl.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[CH2:11]([O:10][C:8](=[O:9])[CH2:7][O:4][CH:2]([CH3:3])[CH3:1])[CH3:12]

参加物

5

反応物 2

HCID 3776IsopropanolHCID 12192Ethyl diazoacetate

生成物 1

HCID 537908Ethyl isopropoxyacetate収率 51.3%

試薬・触媒・溶媒 2

HCID 423677Acetic acid, rhodium salt (4:2)触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-propanol (0.776 mL, 10.0 mmol) in dichloromethane (33 mL) is added rhodium (II) acetate dimer (22 mg) followed by ethyl diazoacetate (1.05 mL, 10.0 mmol). The reaction mixture is stirred at RT for 30 min. The reaction mixture is filtered through Celite, and the filtrate is evaporated and the residue is vacuum distilled at 150° C. to give 750 mg of the product 405. 1H NMR (CDCl3) δ 4.21 (q, 2 H), 4.06 (s, 2 H), 3.73 (m, 1 H), 1.29 (t, 3 H), 1.22 (s, 3 H), 1.19 (s, 3 H); MS: m/z 147 (M++1).

後処理

  1. filtrationThe reaction mixture is filtered through Celite
  2. customthe filtrate is evaporated
  3. distillationdistilled at 150° C.

出典と根拠

ORDレコード
ord-7777b2e233d64c81ae3edec4c6319a78
出典データセット
uspto-grants-2010_06
特許番号
US07741493B2

関連ノート

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