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Hydrochloric Acid → HCID 90449575, 화합물

HRID 1411299
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HRID 1411299 반응식
[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH:17]=[CH:18][O:19]C)[CH:15]=3)[N:10]([C:21]([NH:23][C:24]3[S:25][C:26]([Cl:29])=[CH:27][N:28]=3)=[O:22])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2].Cl.C(=O)([O-])O.[Na+].O>CC(C)=O>[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH2:17][CH:18]=[O:19])[CH:15]=3)[N:10]([C:21]([NH:23][C:24]3[S:25][C:26]([Cl:29])=[CH:27][N:28]=3)=[O:22])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 131732216HCID 131732216, 화합물

생성물 1

HCID 90449575HCID 90449575, 화합물수율 82.2%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
50 °C

실험 절차

1′-Acetyl-N-(5-chlorothiazol-2-yl)-5-(2-methoxyvinyl)spiro[indoline-3,3′-pyrrolidine]-1-carboxamide (83 mg, 0.192 mmol) was dissolved in acetone (3 mL). Thereafter, 6 N hydrochloric acid (1.5 mL) was added to the above obtained solution, and the thus obtained mixture was then stirred at 50° C. for 2 hours. Thereafter, saturated sodium hydrogen carbonate and water were added to the reaction solution, and the mixed solution was then extracted with ethyl acetate. The organic layer was washed with brine, and was then dried over anhydrous sodium sulfate, followed by concentration in vacuo, to obtain 1′-acetyl-N-(5-chlorothiazol-2-yl)-5-(2-oxoethyl)spiro[indoline-3,3′-pyrrolidine]-1-carboxamide (66.1 mg, 82%) in the form of a yellow solid.

후처리

  1. extractionthe mixed solution was then extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialwas then dried over anhydrous sodium sulfate
  4. concentrationfollowed by concentration in vacuo

출처 및 근거

ORD 기록
ord-680bd7613dd64103b310766488ba168b
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921576B2

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