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Cycloheptylamine → 2-Bromo-N-(cycloheptyl)acetamide

HRID 2962
ノート
印刷プレビュー

反応式

HRID 2962 の反応式
[CH:1]1([NH2:8])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(C(C)C)CC)(C)C.[Br:18][CH2:19][C:20](Br)=[O:21]>C(Cl)Cl.O>[Br:18][CH2:19][C:20]([NH:8][CH:1]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 2899CycloheptylamineHCID 61147Bromoacetyl bromideHCID 81531Diisopropylethylamine

生成物 1

HCID 222515742-Bromo-N-(cycloheptyl)acetamide収率 89.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a -20° C. solution of cycloheptylamine (6.37 mL, 50.0 mmol) and diisopropylethylamine (9.58 mL, 55.0 mmol) in methylene chloride (250 mL) was slowly added bromoacetyl bromide (4.78 mL, 55.0 mmol). The reaction mixture was warmed to room temperature over 20 minutes and stirred for an addition 30 minutes. The reaction mixture was diluted with water (100 mL) and stirred for an additional 30 minutes. The organic layer was separated, washed with water (3×100 mL), dried over magnesium sulfate and concentrated in vacuo to afford a beige solid (10.5 g). The crude material was further purified by silica gel flash column chromatography using hexane-ethyl acetate (1:1) as the eluent to give the purified title compound as a whim solid (9.77 g, 83%).

後処理

  1. customTo a -20° C.
  2. stirringstirred for an additional 30 minutes
  3. customThe organic layer was separated
  4. washwashed with water (3×100 mL)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-428799f362c448f9a4b5974ac3fa405b
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05731438

反応ノート

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