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2,6-Xylyl isocyanate → HCID 13137046, 화합물

HRID 1702142
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HRID 1702142 반응식
[CH3:1][C:2]1([CH3:8])[CH2:6][NH:5][C:4](=[S:7])[NH:3]1.[CH3:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH3:16])[C:11]=1[N:17]=[C:18]=[O:19]>CN(C)C=O>[CH3:16][C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([CH3:9])[C:11]=1[NH:17][C:18]([N:5]1[CH2:6][C:2]([CH3:8])([CH3:1])[NH:3][C:4]1=[S:7])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 987872,6-Xylyl isocyanateHCID 30325022-Imidazolidinethione, 4,4-dimethyl-

생성물 1

HCID 13137046HCID 13137046, 화합물수율 55.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 39.0 g (0.3 M) 4,4-dimethylimidazolidine-2-thione, 44.2 g (0.3 M) 2,6-dimethylphenyl isocyanate and 100 ml dimethylformamide was refluxed with stirring for 24 hours. After cooling to room temperature, the solution was filtered from a small amount of insoluble solid and poured into 300 ml water with efficient stirring. The precipitated product was filtered, washed well with water, and dried in vacuo. Yield 62.6 g, mp 228°-231° C. Recrystallization from 600 ml of boiling methanol yielded 46 g of N-(2,6-dimethylphenyl)-4,4-dimethyl-2-thioxo-1-imidazolidinecarboxamide as white crystalline product, mp 241.5°-243° C. A small sample was recrystallized from benzene to give an analytical sample, mp 245.5°-246° C.

후처리

  1. temperaturewas refluxed
  2. filtrationthe solution was filtered from a small amount of insoluble solid
  3. additionpoured into 300 ml water with efficient stirring
  4. filtrationThe precipitated product was filtered
  5. washwashed well with water
  6. customdried in vacuo
  7. customRecrystallization from 600 ml of boiling methanol

출처 및 근거

ORD 기록
ord-519e2a03ac34440788c0284429d76778
출처 데이터셋
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04380548

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