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

HRID 1194798

反応式

HRID 1194798 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 4.34 g (17.5 mmole) of acetoxymethyl 1,3-diacetoxy-2-propyl ether in 45 ml of methylene chloride was stirred at room temperature as a gentle stream of HCl was passed through it. After 2 hours the HCl stream was removed. The flask was stoppered and allowed to stir overnight at room temperature. Then the flask was placed in a water bath at 25°-30°, and the solution was purged with a stream of N2 to remove most of the excess HCl. The remaining solution was concentrated by rotary evaporation. In order to remove traces of HCl, the residual oil was taken up in toluene and concentrated under high vacuum at room temperature. This process was repeated three more times. After vacuum drying at room temperature, the yield of colorless residual oil was 3.83 g (97%). The NMR spectrum indicated complete conversion to product.

後処理

  1. customAfter 2 hours the HCl stream was removed
  2. customThen the flask was placed in a water bath at 25°-30°
  3. customthe solution was purged with a stream of N2
  4. customto remove most of the excess HCl
  5. concentrationThe remaining solution was concentrated by rotary evaporation
  6. customIn order to remove traces of HCl
  7. concentrationconcentrated under high vacuum at room temperature
  8. customAfter vacuum drying at room temperature

出典と根拠

ORDレコード
ord-677037e9ec854a778e240339d12c9f1b
出典データセット
uspto-grants-1989_03
特許番号
US04816447

関連ノート

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