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

HRID 18831

반응식

HRID 18831 반응식
[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]

참가 물질

6

반응물 2

HCID 79001-Methoxy-2-propanolHCID 12192Ethyl diazoacetate

생성물 1

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

시약·촉매·용매 3

HCID 423677Acetic acid, rhodium salt (4:2)촉매HCID 6344Dichloromethane용매HCID 8900Heptane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-6478a7aef5894c6b944da9c656f93df6
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741493B2

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