1-Methoxy-2-propanol → (2-Methoxy-1-methylethoxy)acetic Acid Ethyl Ester

HRID 2053622

反応式

HRID 2053622 の反応式
[CH3:1][O:2][CH2:3][CH:4]([OH:6])[CH3:5].[N+](=[CH:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N-]>ClCCl.CCCCCCC.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[CH2:13]([O:12][C:10](=[O:11])[CH2:9][O:6][CH:4]([CH3:5])[CH2:3][O:2][CH3:1])[CH3:14]

参加物

6

反応物 2

HCID 79001-Methoxy-2-propanolHCID 12192Ethyl diazoacetate

生成物 1

HCID 64044950(2-Methoxy-1-methylethoxy)acetic Acid Ethyl Ester収率 64.9%

試薬・触媒・溶媒 3

HCID 423677Acetic acid, rhodium salt (4:2)触媒HCID 6344Dichloromethane溶媒HCID 8900Heptane溶媒

実験手順

To a solution of 1-methoxy-2-propanol (900 mg, 10.0 mmol) in dichloromethane (20 mL) is added rhodium (II) acetate dimer (10 mg) followed by ethyl diazoacetate (0.95 mL, 9.0 mmol). The reaction mixture is stirred at rt for 30 min. The reaction mixture is diluted with heptane, filtered through celite, and the filtrate is evaporated and the residue is vacuum distilled at 133° C. to give 1.03 g of the product 473. 1H NMR (CDCl3) δ 4.20 (q, 2H), 3.72 (m, 1H), 3.45 (dd, 1H), 3.37 (dd, 1H), 3.35 (s, 3H), 1.27 (t, 3H), 1.19 (d, 3H).

後処理

  1. filtrationfiltered through celite
  2. customthe filtrate is evaporated
  3. distillationdistilled at 133° C.

出典と根拠

ORDレコード
ord-8989f3fb34994c328bd80739944a466c
出典データセット
uspto-grants-2008_02
特許番号
US07326792B2

関連ノート

読み込み中…