Pyridine → HCID 67195545、化合物

HRID 550804ノート

反応式

HRID 550804 の反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[N:10]=[C:11]([N:20]3[CH2:25][CH2:24][CH:23]([OH:26])[CH2:22][CH2:21]3)[C:12]3[CH2:17][S:16](=[O:19])(=[O:18])[CH2:15][C:13]=3[N:14]=2)=[C:4]([F:27])[CH:3]=1.Cl[C:29]([O:31][C:32]1[CH:37]=[CH:36][C:35]([N+:38]([O-:40])=[O:39])=[CH:34][CH:33]=1)=[O:30].N1C=CC=CC=1.[Cl-].[NH4+]>C(Cl)Cl>[C:29](=[O:30])([O:31][C:32]1[CH:33]=[CH:34][C:35]([N+:38]([O-:40])=[O:39])=[CH:36][CH:37]=1)[O:26][CH:23]1[CH2:24][CH2:25][N:20]([C:11]2[C:12]3[CH2:17][S:16](=[O:18])(=[O:19])[CH2:15][C:13]=3[N:14]=[C:9]([C:5]3[CH:6]=[C:7]([F:8])[C:2]([Cl:1])=[CH:3][C:4]=3[F:27])[N:10]=2)[CH2:21][CH2:22]1

参加物

6

反応物 4

HCID 1049PyridineHCID 25517Ammonium ChlorideHCID 821294-Nitrophenyl chloroformateHCID 67199175HCID 67199175、化合物

生成物 1

HCID 67195545HCID 67195545、化合物収率 112.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 571 mg of 1-[2-(4-chloro-2,5-difluorophenyl)-6,6-dioxido-5,7-dihydrothieno[3,4-d]pyrimidin-4-yl]piperidin-4-ol, 0.30 g of 4-nitrophenyl chloroformate, 0.12 ml of pyridine, and 10 ml of methylene chloride was stirred at ambient temperature for 17 hours. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was extracted twice with chloroform. The organic phase was washed with brine, dried over anhydrous magnesium sulfate, and evaporated under reduced pressure to yield 894 mg of 1-[2-(4-chloro-2,5-difluorophenyl)-6,6-dioxido-5,7-dihydrothieno[3,4-d]pyrimidin-4-yl]piperidin-4-yl 4-nitrophenyl carbonate as light yellow solid.

後処理

  1. extractionthe mixture was extracted twice with chloroform
  2. washThe organic phase was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-15f4b1f63a7448899f1aa7f95a1caa04
出典データセット
uspto-grants-2011_05
特許番号
US07947690B2

反応ノート

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