Acetic Acid → HCID 178517893、化合物

HRID 1477566ノート

反応式

HRID 1477566 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 178517893HCID 178517893、化合物収率 99%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 962Water溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0c38336ab92949b691340a14b220604c
出典データセット
uspto-grants-2016_08
特許番号
US09403798B2

反応ノート

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