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

HRID 530208노트

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HRID 530208 반응식
[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(=O)([O-])[O-].[K+].[K+].[CH2:28]([N:30]([CH3:34])[C:31](Cl)=[O:32])[CH3:29]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(#N)C>[I-:1].[CH2:28]([N:30]([CH3:34])[C:31]([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:32])[CH3:29]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 11240471N-Ethyl-N-methylcarbamoyl chlorideHCID 86712421HCID 86712421, 화합물2회

생성물 1

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

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 6342Acetonitrile용매

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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 (0.03 mol) ethyl(methyl)carbamic chloride and 0.1 g of tetrabutylammonium bromide 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 9.5 g of red-brown liquid to be directly used in the next reaction.

후처리

  1. customreact it for 12 hours
  2. temperatureAfter it is cooled to room temperature
  3. filtrationfilter it
  4. customto recover the solvent
  5. customto be directly used in the next reaction

출처 및 근거

ORD 기록
ord-e59c03e08c4843459862ec30a5c6a136
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353049B2

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