Hydrochloric Acid → Chloromethyl 1,3-Diacetoxy-2-propyl Ether

HRID 330587

反応式

HRID 330587 の反応式
[C:1]([O:4][CH2:5][CH:6]([O:12][CH2:13]OC(=O)C)[CH2:7][O:8][C:9](=[O:11])[CH3:10])(=[O:3])[CH3:2].[ClH:18]>C(Cl)Cl>[C:1]([O:4][CH2:5][CH:6]([O:12][CH2:13][Cl:18])[CH2:7][O:8][C:9](=[O:11])[CH3:10])(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 97948881,3-Propanediol, 2-((acetyloxy)methoxy)-, 1,3-diacetate

生成物 1

HCID 19868843Chloromethyl 1,3-Diacetoxy-2-propyl Ether

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 2.33 g (9.4 mmoles) of acetoxymethyl 1,3-diacetoxy-2-propyl ether in 22 ml of sieve-dried methylene chloride was stirred at room temperature while a slow stream of anhydrous hydrogen chloride was passed through the solution. Anhydrous conditions were maintained throughout the reaction. After two hours the reaction was judged to be complete by nuclear magnetic resonance spectroscopy. The reaction mixture was purged with nitrogen and concentrated in vacuo. The residue was taken up in a small volume of toluene and concentrated in vacuo. This was repeated twice and then the residue was pumped in vacuo to remove residual solvent. The yield of chloromethyl 1,3-diacetoxy-2-propyl ether is 1.92 g (91%).

後処理

  1. temperatureAnhydrous conditions were maintained throughout the reaction
  2. customThe reaction mixture was purged with nitrogen
  3. concentrationconcentrated in vacuo
  4. concentrationconcentrated in vacuo
  5. customto remove residual solvent

出典と根拠

ORDレコード
ord-04ea1fadc7c44301bd4af014ed4bcf8c
出典データセット
uspto-grants-1990_01
特許番号
US04897479

関連ノート

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