Sodium Hydroxide → 3-[9-(5-{3-Chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]propanoic acid

HRID 1514289ノート

反応式

HRID 1514289 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[C:27]4[O:26][CH2:25][CH2:24][N:23]([CH2:28][CH2:29][C:30]([O:32]CC)=[O:31])[CH2:22][C:21]=4[CH:20]=[CH:19][CH:18]=3)[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:11])[CH3:10].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[O:16][N:15]=[C:14]([C:17]3[C:27]4[O:26][CH2:25][CH2:24][N:23]([CH2:28][CH2:29][C:30]([OH:32])=[O:31])[CH2:22][C:21]=4[CH:20]=[CH:19][CH:18]=3)[N:13]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH:9]([CH3:11])[CH3:10]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59403533Ethyl 3-[9-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]propanoate

生成物 1

HCID 441292913-[9-(5-{3-Chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]propanoic acid収率 47.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

Ethyl 3-[9-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl]propanoate (Preparation 88) (60 mg, 0.123 mmol) was dissolved in ethanol (5 ml). 2M sodium hydroxide (0.309 ml, 0.617 mmol) was added and the reaction mixture was stirred at 60° C. for 4 h. The solvent was evaporated then the reaction mixture was diluted with water and neutralised with 2M hydrochloric acid and extracted with ethyl acetate. The organic phase was washed with water, dried and evaporated to give the product as a colourless solid (27 mg).

後処理

  1. customThe solvent was evaporated
  2. additionthe reaction mixture was diluted with water and neutralised with 2M hydrochloric acid
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with water
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-624b740c972e4f14b7e5809e21e3eab4
出典データセット
uspto-grants-2012_07
特許番号
US08222245B2

反応ノート

読み込み中…