Dimethylcarbamoyl Chloride → HCID 86737552、化合物

HRID 127212ノート

反応式

HRID 127212 の反応式
[N:1](=[C:3]1[N:7]=[C:6]([CH3:8])[C:5]([CH3:10])([CH3:9])[S:4]1)[OH:2].C(N(CC)CC)C.[CH3:18][N:19]([CH3:23])[C:20](Cl)=[O:21]>COCCOC>[CH3:18][N:19]([CH3:23])[C:20]([O:2][N:1]=[C:3]1[N:7]=[C:6]([CH3:8])[C:5]([CH3:10])([CH3:9])[S:4]1)=[O:21]

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 859972442-Oxo-4,5,5-trimethyl-3-thiazoline oxime

生成物 1

HCID 86737552HCID 86737552、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

15.8 g. (0.1 mol) of 2-oxo-4,5,5-trimethyl-3-thiazoline-oxime and 15.2 g. (0.15 mol) of triethylamine were dissolved in 100 ml. of anhydrous 1,2-dimethoxy-ethane. 16.1 g. (0.15 mol) of dimethylcarbamoyl chloride were added dropwise. The mixture was refluxed for 3 hours and the solvent was distilled off under vacuum. The residue was dissolved in 100 ml. of dichloromethane and washed with water. After the organic phase was dried over sodium sulfate, the solvent was distilled off. The residue was purified chromatographically on silica gel using ether/dichloromethane (9:1) for the elution to yield 2-oxo-4,5,5-trimethyl-3-thiazoline-O-(dimethylcarbamoyl)-oxime, m.p. 108°-110° C.

後処理

  1. temperatureThe mixture was refluxed for 3 hours
  2. distillationthe solvent was distilled off under vacuum
  3. dissolutionThe residue was dissolved in 100 ml
  4. washof dichloromethane and washed with water
  5. dry with materialAfter the organic phase was dried over sodium sulfate
  6. distillationthe solvent was distilled off
  7. customThe residue was purified chromatographically on silica gel
  8. washfor the elution

出典と根拠

ORDレコード
ord-e28039f226eb434b8511f35135413bdf
出典データセット
uspto-grants-1981_03
特許番号
US04255436

反応ノート

読み込み中…