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

HRID 530209ノート

反応式

HRID 530209 の反応式
[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]

参加物

5

反応物 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 86712421HCID 86712421、化合物2 回

生成物 1

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

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ae12098b2e464a6099429a3f82ceb0ca
出典データセット
uspto-grants-2016_05
特許番号
US09353049B2

反応ノート

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