Dimethylcarbamoyl Chloride → HCID 86737552, 화합물

HRID 127212노트

반응식

HRID 127212 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86737552HCID 86737552, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e28039f226eb434b8511f35135413bdf
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255436

반응 노트

불러오는 중…