Triethylamine → 2-Isopropyl-5-methyl-cyclohexanecarboylic acid [2-(2-bromo-phenyl)-ethyl]-amide

HRID 18490

反応式

HRID 18490 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][CH2:5][NH2:6].C(N(CC)CC)C.[CH:18]1([CH3:30])[CH2:23][CH2:22][CH:21]([CH:24]([CH3:26])[CH3:25])[CH:20]([C:27](Cl)=[O:28])[CH2:19]1>C(Cl)Cl>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[CH2:4][CH2:5][NH:6][C:27]([CH:20]1[CH2:19][CH:18]([CH3:30])[CH2:23][CH2:22][CH:21]1[CH:24]([CH3:26])[CH3:25])=[O:28]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27340912-BromophenethylamineHCID 13734319Cyclohexanecarbonyl chloride, 5-methyl-2-(1-methylethyl)-

生成物 1

HCID 668315152-Isopropyl-5-methyl-cyclohexanecarboylic acid [2-(2-bromo-phenyl)-ethyl]-amide収率 98.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A 100 mL round bottom flask equipped with a stir bar was charged with CH2Cl2 (30 mL), 2-bromo-phenethylamine (1.0 g, 5.00 mmol) and triethylamine (684 μl, 5.05 mmol). The reaction solution was treated with menthoyl chloride (1.02 g, 5.05 mmol) in one portion and stirred at ambient temperature for 30 minutes. The reaction was diluted with CH2Cl2 (50 mL) and washed with water (3×100 mL). Organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a thick oil (1.8 g). Product was used for next step without purification.

後処理

  1. customA 100 mL round bottom flask equipped with a stir bar
  2. washwashed with water (3×100 mL)
  3. dry with materialOrganic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1b4ca2bb93d942fea56fb0af7f9c5bd2
出典データセット
uspto-grants-2010_06
特許番号
US07741355B2

関連ノート

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