Trifluoroacetic acid → 1-(2-{2-[(Ethoxycarbonyl)methoxy]-phenyl}-2-oxo-ethyl)-3-methyl-7-(3-methyl-2-buten-1-yl)-8-(3-amino-piperidin-1-yl)-xanthine

HRID 1924412ノート

反応式

HRID 1924412 の反応式
[CH2:1]([O:3][C:4]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14](=[O:47])[CH2:15][N:16]1[C:25](=[O:26])[C:24]2[N:23]([CH2:27][CH:28]=[C:29]([CH3:31])[CH3:30])[C:22]([N:32]3[CH2:37][CH2:36][CH2:35][CH:34]([NH:38]C(OC(C)(C)C)=O)[CH2:33]3)=[N:21][C:20]=2[N:19]([CH3:46])[C:17]1=[O:18])=[O:5])[CH3:2].FC(F)(F)C(O)=O>C(Cl)Cl>[CH2:1]([O:3][C:4]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14](=[O:47])[CH2:15][N:16]1[C:25](=[O:26])[C:24]2[N:23]([CH2:27][CH:28]=[C:29]([CH3:30])[CH3:31])[C:22]([N:32]3[CH2:37][CH2:36][CH2:35][CH:34]([NH2:38])[CH2:33]3)=[N:21][C:20]=2[N:19]([CH3:46])[C:17]1=[O:18])=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 667537501-(2-{2-[(Ethoxycarbonyl)methoxy]-phenyl}-2-oxo-ethyl)-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthine

生成物 1

HCID 100763101-(2-{2-[(Ethoxycarbonyl)methoxy]-phenyl}-2-oxo-ethyl)-3-methyl-7-(3-methyl-2-buten-1-yl)-8-(3-amino-piperidin-1-yl)-xanthine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 209 mg of 1-(2-{2-[(ethoxycarbonyl)methoxy]-phenyl}-2-oxo-ethyl)-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthine in 4 ml methylene chloride is combined with 1 ml of trifluoroacetic acid and stirred for half an hour at ambient temperature. For working up the reaction mixture is diluted with methylene chloride and washed with saturated potassium carbonate solution. The organic phase is dried, evaporated down and chromatographed through a silica gel column with methylene chloride/methanol (1:0 to 4:1) as eluant.

後処理

  1. washwashed with saturated potassium carbonate solution
  2. customThe organic phase is dried
  3. customevaporated down
  4. customchromatographed through a silica gel column with methylene chloride/methanol (1:0 to 4:1) as eluant

出典と根拠

ORDレコード
ord-78b796bc66014ed9a408457ad2b45925
出典データセット
uspto-grants-2012_05
特許番号
US08178541B2

反応ノート

読み込み中…