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Hydrochloric Acid → 1207830-66-7

HRID 655718
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HRID 655718 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 1

HCID 461756111207830-66-7수율 84%

시약·촉매·용매 1

HCID 3776Isopropanol
용매

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-38a18938f2154739a2c9e597a73b66e3
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08071608B2

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