Methanol → HCID 57278482, 화합물

HRID 18814

반응식

HRID 18814 반응식
[CH:1]1([CH2:7][OH:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N+](=[CH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[N-].CO>ClCCl.CCOCC.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:8][CH2:7][CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[CH3:16]

참가 물질

7

반응물 3

HCID 887MethanolHCID 7507CyclohexanemethanolHCID 12192Ethyl diazoacetate

생성물 1

HCID 57278482HCID 57278482, 화합물수율 100.9%

시약·촉매·용매 3

HCID 423677Acetic acid, rhodium salt (4:2)촉매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

To a solution of cyclohexylmethanol (1.23 mL, 10.0 mmol) in dichloromethane (30 mL) is added rhodium (II) acetate dimer (11 mg) followed by ethyl diazoacetate (1.05 mL, 10.0 mmol). The reaction mixture is stirred at RT for 30 min. To the reaction mixture is added MeOH, and the reaction mixture is rotary evaporated, and the residue dissolved in Et2O, filtered through Celite, and the filtrate is evaporated and the residue is vacuum distilled at to give 2.02 g of the product 419. 1H NMR (CDCl3) δ 4.22 (q, 2 H), 4.05 (s, 2 H), 3.33 (d, 2 H), 1.8-1.5 (m, 7 H), 1.4-1.1 (m, 5 H), 1.1-0.9 (m, 2 H); MS: m/z 200 (M++1).

후처리

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

출처 및 근거

ORD 기록
ord-95be94d797e54a1cbb6ae47686dc6060
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741493B2

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