Trifluoroacetic acid → N-(2-[(2,3-Difluorobenzyl)thio]-6-{[(1R,2S)-2,3-dihydroxy-1-methylpropyl]oxy}pyrimidin-4-yl)morpholine-4-sulfonamide

HRID 1175439ノート

反応式

HRID 1175439 の反応式
[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)(=[O:15])=[O:14])[CH:9]=[C:8]([O:22][C@@H:23]([C@@H:25]2[CH2:29][O:28]C(C)(C)[O:26]2)[CH3:24])[N:7]=1.C(O)(C(F)(F)F)=O>CO>[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)(=[O:15])=[O:14])[CH:9]=[C:8]([O:22][C@H:23]([CH3:24])[C@@H:25]([OH:26])[CH2:29][OH:28])[N:7]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 53628371N-(2-[(2,3-Difluorobenzyl)thio]-6-{(1R)-1-[(4S)-2,2-dimethyl-1,3-dioxolan-4-yl]ethoxy}pyrimidin-4-yl)morpholine-4-sulfonamide

生成物 1

HCID 59558812N-(2-[(2,3-Difluorobenzyl)thio]-6-{[(1R,2S)-2,3-dihydroxy-1-methylpropyl]oxy}pyrimidin-4-yl)morpholine-4-sulfonamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of N-(2-[(2,3-difluorobenzyl)thio]-6-{(1R)-1-[(4S)-2,2-dimethyl-1,3-dioxolan-4-yl]ethoxy}pyrimidin-4-yl)morpholine-4-sulfonamide (0.20 g) in MeOH (2 ml) was added TFA (0.4 ml) and the reaction was stirred at room temperature for 20 h. The mixture was evaporated, suspended in saturated sodium carbonate solution and then re-acidified to pH5 with glacial acetic acid with stirring. The resulting solid was collected, washed with H2O and dried to give the title compound as a white solid. Yield 0.15 g.

後処理

  1. customThe mixture was evaporated
  2. stirringre-acidified to pH5 with glacial acetic acid with stirring
  3. customThe resulting solid was collected
  4. washwashed with H2O
  5. customdried

出典と根拠

ORDレコード
ord-0ce3ba0149eb4eba8f9bc5325c52c229
出典データセット
uspto-grants-2010_11
特許番号
US07838675B2

反応ノート

読み込み中…