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Potassium Carbonate → 2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-1,2,3-triazolo(4,5-d)pyrimidin-3-yl)tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl)oxy)ethanol

HRID 1045074
ノート
印刷プレビュー

反応式

HRID 1045074 の反応式
[CH2:1]1[C@@H:3]([NH3+:4])[C@H:2]1[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]([F:12])[CH:6]=1.C1C=CC(C(O)C([O-])=O)=CC=1.C(=O)([O-])[O-].[K+].[K+].Cl[C:31]1[C:32]2[N:43]=[N:42][N:41]([C@H:44]3[C@@H:48]4[O:49][C:50]([CH3:53])([CH3:52])[O:51][C@@H:47]4[C@@H:46]([O:54][CH2:55][CH2:56][OH:57])[CH2:45]3)[C:33]=2[N:34]=[C:35]([S:37][CH2:38][CH2:39][CH3:40])[N:36]=1>O>[F:12][C:7]1[CH:6]=[C:5]([C@@H:2]2[CH2:1][C@H:3]2[NH:4][C:31]2[C:32]3[N:43]=[N:42][N:41]([C@H:44]4[C@@H:48]5[O:49][C:50]([CH3:52])([CH3:53])[O:51][C@@H:47]5[C@@H:46]([O:54][CH2:55][CH2:56][OH:57])[CH2:45]4)[C:33]=3[N:34]=[C:35]([S:37][CH2:38][CH2:39][CH3:40])[N:36]=2)[CH:10]=[CH:9][C:8]=1[F:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 210357742-(((3aR,4S,6R,6aS)-6-(7-Chloro-5-(propylthio)-3H-1,2,3-triazolo(4,5-d)pyrimidin-3-yl)tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl)oxy)ethanolHCID 66808833trans-(1r,2s)-2-(3,4-Difluorophenyl)cyclopropanaminium (2r)-2-hydroxy-2-phenylethanoate

生成物 1

HCID 67289290
2-(((3aR,4S,6R,6aS)-6-(7-(((1R,2S)-2-(3,4-Difluorophenyl)cyclopropyl)amino)-5-(propylthio)-3H-1,2,3-triazolo(4,5-d)pyrimidin-3-yl)tetrahydro-2,2-dimethyl-4H-cyclopenta-1,3-dioxol-4-yl)oxy)ethanol

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

trans-(1R,2S)-2-(3,4-Difluorophenyl)cyclopropanaminium (2R)-2-hydroxy-2-phenylethanoate (258 kg) and potassium carbonate (280 kg) were dissolved in water (1024 kg) and charged to the solution of 2-({(3aR,4S,6R,6aS)-6-[7-chloro-5-(propylthio)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-3-yl]-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl}oxy)ethanol solution from example 5 above with a rate that kept the temperature of the reaction ≦30° C. After full conversion was reached (≧99.9%) the water layer was separated off. The organic layer was washed with a mixture of acetic acid (96 kg) and sodium chloride (96 kg) in water (768 kg) and then washed again with a mixture of acetic acid (32 kg) and sodium chloride (22 kg) in water (952 kg). A third wash of the organic layer was done with sodium chloride (96 kg) in water (864 kg), whereafter the organic layer was used in the next step.

後処理

  1. customthe temperature of the reaction ≦30° C
  2. customwas separated off
  3. washThe organic layer was washed with a mixture of acetic acid (96 kg) and sodium chloride (96 kg) in water (768 kg)
  4. washwashed again with a mixture of acetic acid (32 kg) and sodium chloride (22 kg) in water (952 kg)
  5. washA third wash of the organic layer

出典と根拠

ORDレコード
ord-40bddbef90354835b0dedf9377105dda
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563755B2

反応ノート

読み込み中…

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