p-Toluenesulfonic acid monohydrate → 2-[4-(4-acetyl-3,5-dimethyl-piperazin-1-yl)-phenyl]-5,7-difluoro-3H-quinazolin-4-one

HRID 591598ノート

反応式

HRID 591598 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=1[C:4]([NH2:6])=[O:5].[C:13]([N:16]1[CH:21]([CH3:22])[CH2:20][N:19]([C:23]2[CH:30]=[CH:29][C:26]([CH:27]=O)=[CH:25][CH:24]=2)[CH2:18][CH:17]1[CH3:31])(=[O:15])[CH3:14].S([O-])(O)=O.[Na+].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CN(C)C(=O)C>[C:13]([N:16]1[CH:21]([CH3:22])[CH2:20][N:19]([C:23]2[CH:24]=[CH:25][C:26]([C:27]3[NH:6][C:4](=[O:5])[C:3]4[C:2](=[CH:10][C:9]([F:11])=[CH:8][C:7]=4[F:12])[N:1]=3)=[CH:29][CH:30]=2)[CH2:18][CH:17]1[CH3:31])(=[O:15])[CH3:14]

参加物

6

反応物 4

HCID 521998p-Toluenesulfonic acid monohydrateHCID 23665763Sodium BisulfiteHCID 594419592-Amino-4,6-difluorobenzamideHCID 866620144-(4-Acetyl-3,5-dimethylpiperazin-1-yl)benzaldehyde

生成物 1

HCID 1363480482-[4-(4-acetyl-3,5-dimethyl-piperazin-1-yl)-phenyl]-5,7-difluoro-3H-quinazolin-4-one

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
115 °C

実験手順

To a stirred solution of 2-amino-4,6-difluoro-benzamide (0.66 g, 3.84 mmol) and 4-(4-acetyl-3,5-dimethyl-piperazin-1-yl)-benzaldehyde (1.00 g, 3.84 mmol) in N,N-dimethyl acetamide (20 mL), was added sodium hydrogen sulfite (58.5 wt %, 1.04 g, 5.76 mmol) and p-toluenesulfonic acid monohydrate (0.88 g, 4.61 mmol) and the reaction mixture was stirred at 115° C. for 16 hours. The solvent was evaporated in vacuo, water was added, and the precipitated solid was filtered off, to give 2-[4-(4-acetyl-3,5-dimethyl-piperazin-1-yl)-phenyl]-5,7-difluoro-3H-quinazolin-4-one as a yellow solid, which was used in the next step without further purification.

後処理

  1. customThe solvent was evaporated in vacuo, water
  2. additionwas added
  3. filtrationthe precipitated solid was filtered off

出典と根拠

ORDレコード
ord-3664519c233f4c12955128c86d0b6bc7
出典データセット
uspto-grants-2016_01
特許番号
US09238640B2

反応ノート

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