Water → HCID 15491481、化合物

HRID 567819ノート

反応式

HRID 567819 の反応式
FC(F)(F)C([N:5]([CH2:39][CH2:40][O:41][CH3:42])[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][CH2:14][NH:15][C:16]2[C:21](=[O:22])[N:20]([CH2:23][C:24]([NH:26][CH2:27][C:28]3[CH:29]=[C:30]4[C:34](=[CH:35][CH:36]=3)[NH:33][CH:32]=[C:31]4[CH3:37])=[O:25])[C:19]([CH3:38])=[CH:18][N:17]=2)[CH:8]=1)=O.C(=O)([O-])[O-].[Na+].[Na+].O>CO>[CH3:42][O:41][CH2:40][CH2:39][NH:5][CH2:6][C:7]1[CH:8]=[C:9]([CH:10]=[CH:11][CH:12]=1)[CH2:13][CH2:14][NH:15][C:16]1[C:21](=[O:22])[N:20]([CH2:23][C:24]([NH:26][CH2:27][C:28]2[CH:29]=[C:30]3[C:34](=[CH:35][CH:36]=2)[NH:33][CH:32]=[C:31]3[CH3:37])=[O:25])[C:19]([CH3:38])=[CH:18][N:17]=1

参加物

5

反応物 3

HCID 962WaterHCID 10340Sodium Carbonate2 回HCID 184709502,2,2-Trifluoro-N-(2-methoxyethyl)-N-[3-(2-{[5-methyl-4-(2-{[(3-methyl-1H-indol-5-yl)methyl]amino}-2-oxoethyl)-3-oxo-3,4-dihydro-2-pyrazinyl]amino}ethyl)benzyl]acetamide

生成物 1

HCID 15491481HCID 15491481、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

2,2,2-Trifluoro-N-(2-methoxyethyl)N-[3-(2-{[5-methyl-4-(2-{[(3-methyl-1H-indol-5-yl)methyl]amino}-2-oxoethyl)-3-oxo-3,4-dihydro-2 pyrazinyl]amino}ethyl)benzyl]acetamide (preperation 45) (110 mg, 0.18 mmol) was dissolved in methanol(15 ml) and sodium carbonate solution in water (1.5 ml, 0.765 m, 1.15 mmol) was added. The reaction mixture was stirred for 56 hrs, after which time the reaction was heated to 50° C. and sodium carbonate (1.5 ml, 1.15 mmol) was added. The mixture was heated for 18 hrs and then partitioned between ethyl acetate and water, the organic layer was washed with brine, dried over MgSO4 and the solvent evaporated under reduced pressure. The crude product was triturated with diethyl ether:methanol (1:1) to afford the title compound, 23 mg, (25%).

後処理

  1. temperatureThe mixture was heated for 18 hrs
  2. custompartitioned between ethyl acetate and water
  3. washthe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. customthe solvent evaporated under reduced pressure
  6. customThe crude product was triturated with diethyl ether:methanol (1:1)

出典と根拠

ORDレコード
ord-e334fbf1b04f4609ad450900d8068135
出典データセット
uspto-grants-2001_01
特許番号
US06180627B2

反応ノート

読み込み中…