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Ammonium Chloride → HCID 131732216, 화합물

HRID 1411298
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HRID 1411298 반응식
[Cl-].[CH3:2][O:3][CH2:4][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH3:24]C(C)([O-])C.[K+].[C:30]([N:33]1[CH2:37][CH2:36][C:35]2([C:45]3[C:40](=[CH:41][CH:42]=[C:43](C=O)[CH:44]=3)[N:39]([C:48]([NH:50][C:51]3[S:52][C:53]([Cl:56])=[CH:54][N:55]=3)=[O:49])[CH2:38]2)[CH2:34]1)(=[O:32])[CH3:31].[Cl-].[NH4+]>O1CCCC1.O>[C:30]([N:33]1[CH2:37][CH2:36][C:35]2([C:45]3[C:40](=[CH:41][CH:42]=[C:43]([CH:24]=[CH:4][O:3][CH3:2])[CH:44]=3)[N:39]([C:48]([NH:50][C:51]3[S:52][C:53]([Cl:56])=[CH:54][N:55]=3)=[O:49])[CH2:38]2)[CH2:34]1)(=[O:32])[CH3:31]
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참가 물질

7

반응물 4

HCID 25517Ammonium ChlorideHCID 2723798Methoxymethyl-triphenylphosphonium chlorideHCID 23665647Potassium tert-butoxideHCID 90449869HCID 90449869, 화합물

생성물 1

HCID 131732216HCID 131732216, 화합물수율 78%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

(Methoxymethyl)triphenylphosphonium chloride (0.63 g, 1.85 mmol) was dissolved in tetrahydrofuran (4 mL). Thereafter, potassium tert-butoxide (0.21 g, 1.85 mmol) was added to the above obtained solution under cooling on ice, and the thus obtained mixture was then stirred for 10 minutes. Thereafter, a tetrahydrofuran solution (3 mL) of the 1′-acetyl-N-(5-chlorothiazol-2-yl)-5-formylspiro[indoline-3,3′-pyrrolidine]-1-carboxamide (100 mg, 0.247 mmol) obtained in Step 2 of Example 401 was added to the reaction solution, and the thus obtained mixture was then stirred at room temperature for 1 hour. Thereafter, a saturated aqueous solution of ammonium chloride 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. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=30:1) to obtain 1′-acetyl-N-(5-chlorothiazol-2-yl)-5-(2-methoxyvinyl)spiro[indoline-3,3′-pyrrolidine]-1-carboxamide (83 mg, 78%) in the form of a yellow amorphous product.

후처리

  1. temperatureunder cooling on ice
  2. stirringthe thus obtained mixture was then stirred at room temperature for 1 hour
  3. extractionthe mixed solution was then extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialwas then dried over anhydrous sodium sulfate
  6. concentrationfollowed by concentration in vacuo
  7. customThe obtained residue was purified by silica gel column chromatography (chloroform:methanol=30:1)

출처 및 근거

ORD 기록
ord-6510652329d445b3a845e117c289ac64
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921576B2

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