Hydrochloric Acid → Chloromethyl-3,5-dimethylphenyl chloroformate

HRID 1439423ノート

反応式

HRID 1439423 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712Formaldehyde2 回HCID 6212ChloroformHCID 220261893,5-Xylyl chloroformate

生成物 1

HCID 21397571Chloromethyl-3,5-dimethylphenyl chloroformate

試薬・触媒・溶媒 1

HCID 3007855Zincchloride触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-146e2f64cda94060aae8b9cd36ec8941
出典データセット
uspto-grants-1977_11
特許番号
US04059615

反応ノート

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