Butylamine → 3-(3-Trifluoromethylphenyl)-6-n-butylaminotetrahydro-1,3,5-triazine-2,4-dione

HRID 126760

반응식

HRID 126760 반응식
[CH2:1]([NH2:5])[CH2:2][CH2:3][CH3:4].[F:6][C:7]([F:25])([F:24])[C:8]1[CH:9]=[C:10]([N:14]2[C:19](=[O:20])[NH:18][CH:17](SC)[NH:16][C:15]2=[O:23])[CH:11]=[CH:12][CH:13]=1>C(O)(=O)C>[F:6][C:7]([F:25])([F:24])[C:8]1[CH:9]=[C:10]([N:14]2[C:19](=[O:20])[NH:18][CH:17]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[NH:16][C:15]2=[O:23])[CH:11]=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 8007ButylamineHCID 705459153-(3-Trifluoromethylphenyl)-6-methylthio-tetrahydro-1,3,5-triazine-2,4-dione

생성물 1

HCID 202879633-(3-Trifluoromethylphenyl)-6-n-butylaminotetrahydro-1,3,5-triazine-2,4-dione수율 95%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
145 °C

실험 절차

n-Butylamine (3.92 ml.) was added during 15 minutes to stirred acetic acid (2.4 ml.). After 30 minutes at room temperature, 3-(3-trifluoromethylphenyl)-6-methylthio-tetrahydro-1,3,5-triazine-2,4-dione (6.1 g.) was added to the acetic acid solution. The mixture obtained was then heated at 145° C., for 4 hours. (The liberated methylmercaptan was absorbed into a trap containing an excess of aqueous sodium hydroxide and sodium hypochlorite.) The reaction mixture was cooled to room temperature and then water (75 ml.) was added. The mixture was then stirred for 15 minutes and the white solid which formed was separated by filtration, washed with water (3×150 ml.), and dried (over phosphorus pentoxide) to give 3-(3-trifluoromethylphenyl)-6-n-butylamino-tetrahydro-1,3,5-triazine-2,4-dione (6.0 g., 95%), m.p. 245°-247° C.

후처리

  1. customThe mixture obtained
  2. custom(The liberated methylmercaptan was absorbed into a trap
  3. additioncontaining an excess of aqueous sodium hydroxide and sodium hypochlorite
  4. temperature) The reaction mixture was cooled to room temperature
  5. additionwater (75 ml.) was added
  6. customthe white solid which formed
  7. customwas separated by filtration
  8. washwashed with water (3×150 ml.)
  9. dry with materialdried (over phosphorus pentoxide)

출처 및 근거

ORD 기록
ord-9490e7a2fd5c4ac0930df0f2154a72ac
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254122

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