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

HRID 530208ノート

反応式

HRID 530208 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(=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]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 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 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 6342Acetonitrile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, 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.

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-e59c03e08c4843459862ec30a5c6a136
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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