Hydrochloric Acid → 2-Acetoxyethyl chloromethyl sulfide

HRID 614938

반응식

HRID 614938 반응식
[ClH:1].[C:2]([O:5][CH2:6][CH2:7][SH:8])(=[O:4])[CH3:3].[CH2:9]=O.[Cl-].[Ca+2].[Cl-]>C(Cl)Cl>[Cl:1][CH2:9][S:8][CH2:7][CH2:6][O:5][C:2](=[O:4])[CH3:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 98505Ethanol, 2-mercapto-, 1-acetateHCID 5284359Calcium Chloride

생성물 1

HCID 128996102-Acetoxyethyl chloromethyl sulfide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Hydrogen chloride gas was introduced into a mixture of 2-acetoxyethanethiol (24.0 g) and paraformaldehyde (6.0 g) at a moderate rate with external cooling for 3 hours. Calcium chloride (25 g) was added and the reaction mixture allowed to stand in a salt-ice bath for 4 hours. Methylene chloride (200 ml) was added, the reaction mixture filtered and the solvent evaporated with rigorous exclusion of moisture. The residual oil was distilled to give 2-acetyloxyethyl chloromethyl sulfide (18.5 g, bp 82°-87° C. at 3 mm Hg).

후처리

  1. temperaturewith external cooling for 3 hours
  2. filtrationthe reaction mixture filtered
  3. customthe solvent evaporated with rigorous exclusion of moisture
  4. distillationThe residual oil was distilled

출처 및 근거

ORD 기록
ord-52af1e3fbe744eaab20084b38289c475
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04146715

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