Tetrahydrofuran → Ethyl (2-methoxy-6-nitrophenyl)carbamate

반응식

Cl[C:2]([O:5][C:6](Cl)=[O:7])(Cl)Cl.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[C:12]=1[NH2:20].[CH2:21]1COCC1>>[CH3:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[C:12]=1[NH:20][C:6](=[O:7])[O:5][CH2:2][CH3:21]

참가 물질

반응물 3

HCID 8028Tetrahydrofuran

HCID 10426Diphosgene

HCID 854916-Nitro-o-anisidine

생성물 1

HCID 86603972Ethyl (2-methoxy-6-nitrophenyl)carbamate

실험 절차

17.1 mL (0.141 mol) trichloromethylchloroformate are added dropwise at reflux temperature to a solution of 23.8 g (0.142 mol) 2-methoxy-6-nitro-phenylamine in 300 mL THF and then the mixture is stirred for 4 hours at this temperature. The solvent is distilled off and the residue is stirred with isopropanol, during which time a yellow solid is precipitated. Yield: 25.0 g (73%); mass spectroscopy: [M+H]+=241.

후처리

distillationThe solvent is distilled off
stirringthe residue is stirred with isopropanol, during which time a yellow solid
customis precipitated

출처 및 근거

ORD 기록: ord-5731544a9aa245a3966584cf36fb4237
출처 데이터셋: uspto-grants-2008_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07429583B2

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