Triphenylphosphine → HCID 67001595, 화합물

HRID 2191582노트

반응식

HRID 2191582 반응식
[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]([CH2:14][OH:15])[C:9]([CH3:13])([CH3:12])[CH2:10]O)([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[C:1]([O:5][C:6](=[O:16])[NH:7][CH:8]1[C:9]([CH3:13])([CH3:12])[CH2:10][O:15][CH2:14]1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 11776Triphenylphosphine2회HCID 73096807HCID 73096807, 화합물

생성물 1

HCID 67001595HCID 67001595, 화합물수율 74%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(3-Hydroxy-1-hydroxymethyl-2,2-dimethyl-propyl)-carbamic acid tert-butyl ester (104 mg, 0.44 mmol) was dissolved in dichloromethane (2.2 mL). Triphenylphosphine (0.115 g, 0.44 mmol) was added followed by azodiethylcarboxylate (0.16 mL, 0.88 mmol). After 30 min additional triphenylphosphine (0.115 g, 0.44 mmol) and azodiethylcarboxylate (0.16 mL, 0.88 mmol) were added and the reaction mixture was stirred for 72 h. The solvent was evaporated and the residue purified by silica gel chromatography (ethyl acetate/hexanes) to give 70 mg (74%) of (4,4-dimethyl-tetrahydro-furan-3-yl)-carbamic acid tert-butyl ester.

후처리

  1. customThe solvent was evaporated
  2. customthe residue purified by silica gel chromatography (ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-8944090ef8fe48e2bf7373bbd6eebcb2
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329699B2

반응 노트

불러오는 중…