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Pyridine → Acetic acid, chloro-, isobutyl ester

HRID 492136
ノート
印刷プレビュー

反応式

HRID 492136 の反応式
[Cl:1][CH2:2][C:3](Cl)=[O:4].[CH3:6][CH:7]([CH3:10])[CH2:8][OH:9].N1C=CC=CC=1>C(OCC)C>[Cl:1][CH2:2][C:3]([O:9][CH2:8][CH:7]([CH3:10])[CH3:6])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 6560IsobutanolHCID 6577Chloroacetyl chloride

生成物 1

HCID 139442Acetic acid, chloro-, isobutyl ester収率 94%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of chloroacetyl chloride (3.2 mL, 40 mmol) in anhydrous diethyl ether (20 mL) was added dropwise within 1 h to a solution of 2-methylpropanol (2.96 g, 40 mmol) and pyridine (3.25 mL, 40 mmol) in anhydrous diethyl ether (80 mL) at 0° C. After warming to RT, the white suspension was stirred for 3 h. The precipitate was removed by filtration and washed by diethyl ether (15 mL). The combined organic solution was washed with HCl (2 N, 30 mL), followed by sat. NaHCO3 (30 mL), sat. NaCl (30 mL) solutions and dried with Na2SO4. Removal of the solvent at about 60 mmHg/30° C. afford 2-Methylpropyl Chloroacetate (5.65 g, 94%) which was used without further purification.

後処理

  1. customThe precipitate was removed by filtration
  2. washwashed by diethyl ether (15 mL)
  3. washThe combined organic solution was washed with HCl (2 N, 30 mL)
  4. dry with materialdried with Na2SO4
  5. customRemoval of the solvent at about 60 mmHg/30° C.

出典と根拠

ORDレコード
ord-d50588ba572f42499f258e9c04f6cbd1
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531662B2

反応ノート

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