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Water → tert-Butyl 4-(3-chloropropyl)piperazine-1-carboxylate

HRID 1618810
ノート
印刷プレビュー

反応式

HRID 1618810 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH2:15][CH2:16][CH2:17][Cl:18].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:15][CH2:16][CH2:17][Cl:18])[CH2:10][CH2:9]1)([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 53412057tert-Butyl 4-(3-chloropropyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

To a solution of 4.94 g tert-Butyl-1-piperazine-carboxylate and 12.66 g 1-Bromo-3-chloropropane in 15 ml DMF (dry) was added 4.08 g K2CO3 and the reaction heated to 50° C. for one minute and stirred at room temperature for additional 3 h. The reaction mixture is pored into 200 ml of water and extracted with DCM. The combined organic phases were washed with water and dried over MgSO4 and evaporated in vacuo. The product was purified by flash column chromatography (n-heptane/ethylacetate 1:1, RF=0.3) Yield 3.9 g.

後処理

  1. extractionextracted with DCM
  2. washThe combined organic phases were washed with water
  3. dry with materialdried over MgSO4
  4. customevaporated in vacuo
  5. customThe product was purified by flash column chromatography (n-heptane/ethylacetate 1:1, RF=0.3) Yield 3.9 g

出典と根拠

ORDレコード
ord-49e44022ee1a44cb8badb5318fca757a
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08771644B2

反応ノート

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