Water → HCID 59625636、化合物

HRID 2192811ノート

反応式

HRID 2192811 の反応式
C([O:4][CH2:5][CH:6]1[CH2:11][CH:10]([N:12]([C:17]([C:19]2[C:20]([NH:29][CH2:30][C:31]3[O:32][CH:33]=[CH:34][CH:35]=3)=[N:21][C:22]([C:25]([CH3:28])([CH3:27])[CH3:26])=[N:23][CH:24]=2)=[O:18])[CH2:13][CH:14]([CH3:16])[CH3:15])[CH2:9][N:8]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[CH2:7]1)(=O)C.O.[OH-].[Na+]>CO>[C:25]([C:22]1[N:21]=[C:20]([NH:29][CH2:30][C:31]2[O:32][CH:33]=[CH:34][CH:35]=2)[C:19]([C:17]([N:12]([CH2:13][CH:14]([CH3:16])[CH3:15])[CH:10]2[CH2:11][CH:6]([CH2:5][OH:4])[CH2:7][N:8]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[CH2:9]2)=[O:18])=[CH:24][N:23]=1)([CH3:28])([CH3:27])[CH3:26]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 59625506HCID 59625506、化合物

生成物 1

HCID 59625636HCID 59625636、化合物収率 97.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

To a solution of tert-butyl 3-[(acetyloxy)methyl]-5-[({2-tert-butyl-4-[(furan-2-ylmethyl)amino]pyrimidin-5-yl}carbonyl)(2-methylpropyl)amino]piperidine-1-carboxylate (780 mg) in methanol (10 ml)-water (9 ml) was added 8 M aqueous sodium hydroxide solution (0.83 ml), and the mixture was stirred at 70° C. for 7 hr and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and the fraction eluted with ethyl acetate-hexane (5:95-100:0) was concentrated under reduced pressure to give the object compound (709 mg).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. washthe fraction eluted with ethyl acetate-hexane (5:95-100:0)
  6. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-9a1363dc62074ebe8efc00fc45839e6e
出典データセット
uspto-grants-2012_12
特許番号
US08329691B2

反応ノート

読み込み中…