Phenyl Isothiocyanate → HCID 54237642, 화합물

HRID 647584노트

반응식

HRID 647584 반응식
C[O-].[Na+].I.[NH:5]=[C:6]1[N:10]([CH3:11])[CH:9]=[CH:8][S:7]1.[C:12]1([N:18]=[C:19]=[S:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(O)C.C1(C)C=CC=CC=1>[CH3:11][N:10]1[CH:9]=[CH:8][S:7][C:6]1=[N:5][C:19]([NH:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[S:20]

참가 물질

6

반응물 3

HCID 7673Phenyl IsothiocyanateHCID 10942334Sodium MethoxideHCID 429153603-METHYL-1,3-THIAZOL-2(3H)-IMINE HYDROIODIDE

생성물 1

HCID 54237642HCID 54237642, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 1140Toluene용매

실험 절차

Sodium methoxide (5.40 g) was added to a stirred mixture of 2-imino-3-methylthiazoline hydroiodide (24.95 g) in ethanol (100 ml) and the mixture brought to reflux. Phenyl isothiocyanate (16.35 g) in toluene (50 ml) was added over 30 minutes and reflux continued for a further hour then cooled in ice. The solid obtained on filtration and washing with ethanol and water was dried to give the product, mpt 172.5°-173.5°. Recrystallisation from iso-propanol gave analytically pure product, mpt 173.5°-174°.

후처리

  1. temperatureto reflux
  2. temperaturereflux
  3. waitcontinued for a further hour
  4. temperaturethen cooled in ice
  5. customThe solid obtained on filtration
  6. washwashing with ethanol and water
  7. customwas dried
  8. customto give the product, mpt 172.5°-173.5°
  9. customRecrystallisation from iso-propanol
  10. customgave analytically pure product, mpt 173.5°-174°

출처 및 근거

ORD 기록
ord-2dd75946f83a4ef09305d7039efdd6e7
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409216

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