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Nitromethane → HCID 86653260, 화합물

HRID 2196648
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HRID 2196648 반응식
[Cl-].[Cl-].[Cl-].[Al+3].C[N+]([O-])=O.[F:9][C:10]1[C:27]([NH:28][S:29]([CH2:32][CH2:33][CH3:34])(=[O:31])=[O:30])=[CH:26][CH:25]=[C:24]([F:35])[C:11]=1[C:12]([NH:14][C:15]1[CH:16]=[C:17]2[CH:23]=[CH:22][NH:21][C:18]2=[N:19][CH:20]=1)=[O:13].[Cl:36][CH2:37][C:38](Cl)=[O:39]>C(Cl)Cl.[Cl-].[NH4+]>[Cl:36][CH2:37][C:38]([C:23]1[C:17]2[C:18](=[N:19][CH:20]=[C:15]([NH:14][C:12](=[O:13])[C:11]3[C:24]([F:35])=[CH:25][CH:26]=[C:27]([NH:28][S:29]([CH2:32][CH2:33][CH3:34])(=[O:31])=[O:30])[C:10]=3[F:9])[CH:16]=2)[NH:21][CH:22]=1)=[O:39]
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참가 물질

7

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HCID 6375Nitromethane2회HCID 6577Chloroacetyl chloride2회HCID 6451240Aluminum(III) ChlorideHCID 441994082,6-difluoro-3-(propylsulfonamido)-N-(1H-pyrrolo[2,3-b]pyridin-5-yl)benzamide

생성물 1

HCID 86653260HCID 86653260, 화합물수율 50%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
3회
HCID 25517Ammonium Chloride용매

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온도
0 °C

실험 절차

A solution of aluminum trichloride (0.266 g, 2.00 mmol) in 1:1 DCM:CH3NO2 (5 mL) was added slowly to a slurry of 2,6-difluoro-3-(propylsulfonamido)-N-(1H-pyrrolo[2,3-b]pyridin-5-yl)benzamide (0.100 g, 0.254 mmol) in 1:1 DCM:CH3NO2 (2 mL) at 0° C. The solution was stirred at 0° C. for 40 minutes. A solution of 2-chloroacetyl chloride (0.0307 mL, 0.380 mmol) in DCM (1 mL) was added, and the reaction mixture was allowed to warm to room temperature overnight. Additional 2-chloroacetyl chloride (5 eq.) was added, and the reaction mixture was warmed to 50° C. for 20 hours. The solution was cooled and diluted with saturated aqueous ammonium chloride and extracted with EtOAc (3 X). The organic layers were dried over Na2SO4, filtered and concentrated under reduced pressure. They were then purified via column chromatography (5% MeOH/DCM) to afford N-(3-(2-chloroacetyl)-1H-pyrrolo[2,3-b]pyridin-5-yl)-2,6-difluoro-3-(propylsulfonamido)benzamide (59 mg, 50%) as a solid.

후처리

  1. customat 0° C
  2. temperatureto warm to room temperature overnight
  3. temperaturethe reaction mixture was warmed to 50° C. for 20 hours
  4. temperatureThe solution was cooled
  5. extractionextracted with EtOAc (3 X)
  6. dry with materialThe organic layers were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThey were then purified via column chromatography (5% MeOH/DCM)

출처 및 근거

ORD 기록
ord-8ba30353c9bd4c4391a00059310848a0
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08338452B2

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