Acetic Acid → HCID 178517893, 화합물

HRID 1477566노트

반응식

HRID 1477566 반응식
C(O)(=O)C.Cl[C:6]1[NH:11][C:10](=[O:12])[N:9]=[C:8]([N:13]2[CH2:18][CH2:17][N:16]([C:19]3[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=3)[CH2:15][CH2:14]2)[N:7]=1>[OH-].[Pd+2].[OH-].O>[F:25][C:22]1[CH:23]=[CH:24][C:19]([N:16]2[CH2:15][CH2:14][N:13]([C:8]3[N:7]=[CH:6][NH:11][C:10](=[O:12])[N:9]=3)[CH2:18][CH2:17]2)=[CH:20][CH:21]=1

참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 1369330476-Chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one

생성물 1

HCID 178517893HCID 178517893, 화합물수율 99%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 962Water용매

실험 절차

An acetic acid (15 mL)-water (35 mL) mixed solution of 6-chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one (1.00 g, 3.23 mmol) synthesized in Reference Synthesis Example 2 and palladium hydroxide-activated carbon catalyst (100 mg) was stirred under hydrogen atmosphere at room temperature for 3 days. After completion of the reaction, the reaction solution was filtered with Celite and the filtered residue was washed with methanol, followed by concentrating the obtained solution under reduced pressure. Toluene was added to the residue and the mixture was azeotropically dehydrated four times. The obtained residue was dried under reduced pressure to obtain the title compound (876 mg, yield 99%).

후처리

  1. customAfter completion of the reaction
  2. filtrationthe reaction solution was filtered with Celite
  3. washthe filtered residue was washed with methanol
  4. concentrationby concentrating the obtained solution under reduced pressure
  5. additionToluene was added to the residue
  6. customThe obtained residue was dried under reduced pressure

출처 및 근거

ORD 기록
ord-0c38336ab92949b691340a14b220604c
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403798B2

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