Acetonitrile → (S)-1-(3-(ethyl(methyl)carbamoyloxy)phenyl)-N,N-dimethyl-N-((S)-1-phenylethyl)ethanaminium iodide

HRID 530209노트

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[I-:1].[OH:2][C:3]1[CH:4]=[C:5]([C@@H:9]([N+:11]([CH3:21])([CH3:20])[C@H:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])[CH3:10])[CH:6]=[CH:7][CH:8]=1.[C:22](=[O:25])([O-])[O-].[K+].[K+].C1O[CH2:44][CH2:43]OCCOCCOCCOCCOC1.[C:46](#[N:48])C>>[I-:1].[CH2:43]([N:48]([CH3:46])[C:22]([O:2][C:3]1[CH:4]=[C:5]([C@@H:9]([N+:11]([CH3:21])([CH3:20])[C@H:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])[CH3:10])[CH:6]=[CH:7][CH:8]=1)=[O:25])[CH3:44]

참가 물질

반응물 4

HCID 6342Acetonitrile

HCID 11430Potassium Carbonate

HCID 2855718-Crown-6

HCID 86712421HCID 86712421, 화합물2회

생성물 1

HCID 86712425(S)-1-(3-(ethyl(methyl)carbamoyloxy)phenyl)-N,N-dimethyl-N-((S)-1-phenylethyl)ethanaminium iodide

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온도: 60 °C

실험 절차

Mix 7.9 g (0.02 mol) of(S)-1-(3-hydroxyphenyl)-N,N-dimethyl-N—((S)-1-phenylethyl)ethanaminium iodide (formula VIII) with 180 ml of acetonitrile, 4.1 g (0.03 mol) of potassium carbonate, 3.6 g (0.03 mol) ethyl(methyl)carbamic chloride chloride and 0.1 g 18-crown-6 at room temperature, heat it to 60° C. and react it for 12 hours. After it is cooled to room temperature, filter it and reduce the pressure to recover the solvent and receive 9.9 g of red-brown liquid to be directly used in the next reaction.

후처리

customreact it for 12 hours
temperatureAfter it is cooled to room temperature
filtrationfilter it
customto recover the solvent
customto be directly used in the next reaction

출처 및 근거

ORD 기록: ord-ae12098b2e464a6099429a3f82ceb0ca
출처 데이터셋: uspto-grants-2016_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09353049B2

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