Sulfuric Acid → p-Tolylthiourea

HRID 1769018

반응식

HRID 1769018 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.S(=O)(=O)(O)O.[S-:14][C:15]#[N:16].[NH4+].O.N>C1(C)C=CC=CC=1>[CH3:8][C:5]1[CH:6]=[CH:7][C:2]([NH:1][C:15]([NH2:16])=[S:14])=[CH:3][CH:4]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric Acid2회HCID 7813p-ToluidineHCID 15666Ammonium thiocyanateHCID 12896473Azane;hydrate

생성물 1

HCID 722833p-Tolylthiourea수율 78.5%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
75 °C

실험 절차

10.7 g of 4-toluidine was added dropwise to 27% aqueous sulfuric acid solution which contains 5.4 g of sulfuric acid. After the reaction mixture was heated to 75° C., 8.4 g of ammonium thiocyanate in a solid state was slowly added thereto. Upon complete addition, the reaction mixture was stirred for 20 hours at 80° C. to 90° C. After adding toluene, the whole mixture was refluxed for one hour, cooled to room temperature and then adjusted to pH 7.5 to 8 by slowly adding ammonia water. The resulting white solid was filtered, washed once with each of water and toluene and then dried under reduced pressure to obtain the title compound as a white solid (Yield: 78.5%).

후처리

  1. additionUpon complete addition
  2. temperaturethe whole mixture was refluxed for one hour
  3. temperaturecooled to room temperature
  4. filtrationThe resulting white solid was filtered
  5. washwashed once with each of water and toluene
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-b9b8b619343f4e90b7e36e946562ce05
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380735

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