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

HRID 1194798

반응식

HRID 1194798 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-677037e9ec854a778e240339d12c9f1b
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04816447

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