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Ethyl diazoacetate → Ethyl (dicyclopropylmethoxy)acetate

HRID 2053614
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HRID 2053614 반응식
[CH:1]1([CH:4]([CH:6]2[CH2:8][CH2:7]2)[OH:5])[CH2:3][CH2:2]1.[N+](=[CH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[N-]>ClCCl.CCCCCCC.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[CH2:15]([O:14][C:12](=[O:13])[CH2:11][O:5][CH:4]([CH:6]1[CH2:8][CH2:7]1)[CH:1]1[CH2:3][CH2:2]1)[CH3:16]
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참가 물질

6

반응물 2

HCID 12192Ethyl diazoacetateHCID 84336Dicyclopropylmethanol

생성물 1

HCID 22159734Ethyl (dicyclopropylmethoxy)acetate수율 52.1%

시약·촉매·용매 3

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

실험 절차

To a solution of dicyclopropylmethan-1-ol (1.5 mL, 12.7 mmol) in dichloromethane (20 mL) is added rhodium (II) acetate dimer (10 mg) followed by ethyl diazoacetate (1.26 mL, 12.0 mmol). The reaction mixture is stirred at rt for 48 h. The reaction mixture is diluted with heptane, and filtered. The filtrate is evaporated, and the residue is vacuum distilled at 170° C. to give 1.24 g of the product 448.

후처리

  1. filtrationfiltered
  2. customThe filtrate is evaporated
  3. distillationdistilled at 170° C.

출처 및 근거

ORD 기록
ord-1ee906f44b5d40449982e193446f75ca
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07326792B2

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