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Dimethylamine → Thiourea, N'-(3-hydroxyphenyl)-N,N-dimethyl-

HRID 1076288
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HRID 1076288 반응식
[OH:1][C:2]1[CH:3]=[C:4]([N:8]=[C:9]=[S:10])[CH:5]=[CH:6][CH:7]=1.[C:11]([NH:15][C:16](=[O:18])[O-:17])([CH3:14])([CH3:13])[CH3:12].CNC>CO>[OH:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]([N:15]([CH3:16])[CH3:11])=[S:10])[CH:5]=[CH:6][CH:7]=1.[C:11]([NH:15][C:16](=[O:17])[O-:18])([CH3:14])([CH3:13])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 674DimethylamineHCID 8200263-isothiocyanatophenolHCID 21252905Tert-butylcarbamate

생성물 2

HCID 5368133Thiourea, N'-(3-hydroxyphenyl)-N,N-dimethyl-HCID 21252905Tert-butylcarbamate

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
15 °C

실험 절차

1-(meta-hydroxyphenyl)-3,3-dimethyl-2-thiourea, tertbutylcarbamate is prepared by charging to a suitable vessel about 25 g. (approximately 0.1 mole) meta-hydroxyphenyl isothiocyanate, tert-butylcarbamate dissolved in about 150 ml. of methanol, and adding, with stirring about 154 g. (approximately 0.12 moles) of 40 percent aqueous dimethylamine mixed with about 50 ml. of methanol in a single increment. The mass quickly solidifies as the temperature rises from about room temperature to about 60°C. The mass is cooled to about 15°C., separated from the residual liquid by filtration, washed with four 150 ml. portions of a 75 percent methanol/25 percent water solution and dried under vacuum overnight.

후처리

  1. customby charging to a suitable vessel
  2. customrises from about room temperature to about 60°C
  3. customseparated from the residual liquid by filtration
  4. washwashed with four 150 ml
  5. dry with materialportions of a 75 percent methanol/25 percent water solution and dried under vacuum overnight

출처 및 근거

ORD 기록
ord-6d39d2c9fa2743f29cca32e1a8c46bdf
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03956384

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