Hydrochloric Acid → Chloromethyl-3,5-dimethylphenyl chloroformate

HRID 1439423노트

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HRID 1439423 반응식
[Cl:1][C:2]([O:4][C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([CH3:12])[CH:6]=1)=[O:3].C=O.Cl.[CH:16](Cl)(Cl)[Cl:17]>[Cl-].[Zn+2].[Cl-]>[Cl:1][C:2]([O:4][C:5]1[CH:6]=[C:7]([CH3:12])[CH:8]=[C:9]([CH3:11])[C:10]=1[CH2:16][Cl:17])=[O:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712Formaldehyde2회HCID 6212ChloroformHCID 220261893,5-Xylyl chloroformate

생성물 1

HCID 21397571Chloromethyl-3,5-dimethylphenyl chloroformate

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

실험 절차

Into a stirred mixture of 37 parts of 3,5-xylenyl chloroformate, 78 parts of paraformaldehyde, 10 parts of powdered anhydrous zinc chloride, and 150 parts of chloroform at 20-30 degrees, was passed hydrogen chloride gas over 101/2 hours. The paraformaldehyde slowly dissolved. Then the reaction mixture was agitated briefly with ice water, after which the organic layer was decanted, dried over magnesium sulfate, filtered, and solvent was evaporated off. The residual liquid was distilled to obtain 17 parts of chloromethyl-3,5-dimethylphenyl chloroformate, boiling point 80° - 85° (0.005 millimeter), in which the position of the chloromethyl group is indicated to be mostly para by NMR analysis.

후처리

  1. custom2 hours
  2. customafter which the organic layer was decanted
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customsolvent was evaporated off
  6. distillationThe residual liquid was distilled

출처 및 근거

ORD 기록
ord-146e2f64cda94060aae8b9cd36ec8941
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04059615

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