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

HRID 1024934ノート

反応式

HRID 1024934 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-e7a2584945504fe8a4566a1bf21607ba
出典データセット
uspto-grants-2014_05
特許番号
US08722883B2

反応ノート

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