Methanol → HCID 86686238、化合物

HRID 1021287ノート

反応式

HRID 1021287 の反応式
[Si:1]([O:8][CH2:9][C:10]1[C:11]([F:33])=[C:12]([C:16]2[CH:17]=[N:18][C:19]([N:22]3[CH2:27][CH2:26][N:25]([S:28]([CH:31]=[CH2:32])(=[O:30])=[O:29])[CH2:24][CH2:23]3)=[N:20][CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C1C[O:37][CH2:36]C1.CO.[OH-].[Na+]>C(Cl)(Cl)Cl>[Si:1]([O:8][CH2:9][C:10]1[C:11]([F:33])=[C:12]([C:16]2[CH:17]=[N:18][C:19]([N:22]3[CH2:23][CH2:24][N:25]([S:28]([CH2:31][CH2:32][O:37][CH3:36])(=[O:30])=[O:29])[CH2:26][CH2:27]3)=[N:20][CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:6])([CH3:7])[CH3:5])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 86686239HCID 86686239、化合物

生成物 1

HCID 86686238HCID 86686238、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

5-[3-({[tert-Butyl(dimethyl)silyl]oxy}methyl)-2-fluorophenyl]-2-[4-(vinylsulfonyl)piperazin-1-yl]pyrimidine (360 mg) was mixed with THF (3 ml) and MeOH (4 ml), and a 1 M aqueous NaOH solution (1.46 ml) was added thereto, followed by stirring at room temperature for 3 hours. CHCl3 was added to the reaction mixture, which was washed with water and saturated brine, and dried over Na2SO4. Then, the organic layer was concentrated under reduced pressure to obtain 5-[3-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-fluorophenyl]-2-{4-[(2-methoxyethyl)sulfonyl]piperazin-1-yl}pyrimidine (353 mg).

後処理

  1. washwas washed with water and saturated brine
  2. dry with materialdried over Na2SO4
  3. concentrationThen, the organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-acd1d673abf74ef0a902453482dde447
出典データセット
uspto-grants-2014_05
特許番号
US08716470B2

反応ノート

読み込み中…