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Hydrochloric Acid → 1207830-66-7

HRID 655718
ノート
印刷プレビュー

反応式

HRID 655718 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]#[N:10])[C:4]=1[N:11]1[C:15]2=[N:16][CH:17]=[N:18][C:19]([O:20][C@@H:21]([CH2:32][O:33][C@H:34]([CH3:47])[CH2:35][O:36][Si](C(C)C)(C(C)C)C(C)C)[C:22]([NH:24][C:25]3[CH:30]=[N:29][C:28]([CH3:31])=[CH:27][N:26]=3)=[O:23])=[C:14]2[CH:13]=[N:12]1.C(=O)(O)[O-].[Na+]>CC(O)C>[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]#[N:10])[C:4]=1[N:11]1[C:15]2[N:16]=[CH:17][N:18]=[C:19]([O:20][C@@H:21]([CH2:32][O:33][C@H:34]([CH3:47])[CH2:35][OH:36])[C:22]([NH:24][C:25]3[CH:30]=[N:29][C:28]([CH3:31])=[CH:27][N:26]=3)=[O:23])[C:14]=2[CH:13]=[N:12]1
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 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 46938169(2S)-2-(1-(2-chloro-6-cyanophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-N-(5-methylpyrazin-2-yl)-3-((R)-1-(triisopropylsilyloxy)propan-2-yloxy)propanamide

生成物 1

HCID 461756111207830-66-7収率 84%

試薬・触媒・溶媒 1

HCID 3776Isopropanol
溶媒

実験手順

Hydrochloric acid (6M, 4 equivs) was added with stirring to a solution of (2S)-2-(1-(2-chloro-6-cyanophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-N-(5-methylpyrazin-2-yl)-3-((R)-1-(triisopropylsilyloxy)propan-2-yloxy)propanamide (Intermediate AZ1) (1 equiv) in propan-2-ol (9 rel vols) in an inert atmosphere at ambient temperature. The mixture was stirred for 6 hours then basified carefully with aqueous sodium bicarbonate solution. The volume was reduced to half of the original volume by distillation under reduced pressure and then ethyl acetate and water were added. The mixture was stirred and then the phases were separated. The aqueous phase was extracted with ethyl acetate and the combined organic extract and washings were dried by azeotropic distillation. The product was crystallised from a mixture of ethyl acetate/heptane (5:6 vols). Yield 84%.

後処理

  1. distillationThe volume was reduced to half of the original volume by distillation under reduced pressure
  2. additionethyl acetate and water were added
  3. stirringThe mixture was stirred
  4. customthe phases were separated
  5. extractionThe aqueous phase was extracted with ethyl acetate
  6. extractionthe combined organic extract
  7. customwashings were dried by azeotropic distillation
  8. customThe product was crystallised from a mixture of ethyl acetate/heptane (5:6 vols)

出典と根拠

ORDレコード
ord-38a18938f2154739a2c9e597a73b66e3
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071608B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート