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

HRID 530211노트

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HRID 530211 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(#N)C.[OH-].[K+].[CH2:27]([N:29]([CH3:33])[C:30](Cl)=[O:31])[CH3:28]>C(O)CO>[I-:1].[CH2:27]([N:29]([CH3:33])[C:30]([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:31])[CH3:28]

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 14797Potassium HydroxideHCID 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 1

HCID 174Ethylene Glycol용매

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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, 1.7 g (0.03 mol) of potassium hydroxide, 3.6 (0.03 mol) ethyl(methyl)carbamic chloride and 0.1 g of macrogol 400 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 10.2 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-d4ff81d75b4f457b999f564a9d9c2c6c
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353049B2

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