a-(acetyloxy)-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide → (+/-)alpha-Hydroxy-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

HRID 3595ノート

反応式

HRID 3595 の反応式
C([O:4][CH:5]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[CH2:21][N:20]3[CH:28]=[CH:29][CH:30]=[C:19]3[CH2:18]2)=[O:16])=[CH:11][CH:10]=1)=[O:7])(=O)C>[OH-].[Na+].CO.O>[OH:4][CH:5]([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[CH2:21][N:20]3[CH:28]=[CH:29][CH:30]=[C:19]3[CH2:18]2)=[O:16])=[CH:11][CH:10]=1)=[O:7]

参加物

5

実験手順

A solution of 0.34 g of α-(acetyloxy)-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide in 2 ml of 1N NaOH and 4 ml of methyl alcohol is stirred at room temperature for 30 minutes, diluted with 2 ml of water and evaporated in vacuo. The aqueous suspension is extracted with 30 ml of ethyl acetate and the extract washed with brine, dried with Na2SO4 and filtered through a pad of hydrous magnesium silicate and evaporated in vacuo to a residue. The residue is stirred with ether-hexanes to give 0.26 g of cream colored solid. MS(CI): 438(M+H).

後処理

  1. customevaporated in vacuo
  2. extractionThe aqueous suspension is extracted with 30 ml of ethyl acetate
  3. washthe extract washed with brine
  4. dry with materialdried with Na2SO4
  5. filtrationfiltered through a pad of hydrous magnesium silicate
  6. customevaporated in vacuo to a residue
  7. customto give 0.26 g of cream

出典と根拠

ORDレコード
ord-9bad5fecb8854a0b85e3651c3a658f21
出典データセット
uspto-grants-1998_03
特許番号
US05733905

反応ノート

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