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

HRID 530211ノート

反応式

HRID 530211 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(#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]

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 14797Potassium HydroxideHCID 11240471N-Ethyl-N-methylcarbamoyl chlorideHCID 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

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

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, 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.

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-d4ff81d75b4f457b999f564a9d9c2c6c
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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