9-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrile → HCID 16065358, 화합물

HRID 240309

반응식

HRID 240309 반응식
Cl.[F:2][C:3]1([F:9])[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.[O:10]=[C:11]1[C:23]2[C:18](=[N:19][C:20](C#N)=[C:21]([C:24]#[N:25])[N:22]=2)[C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]1=2>[OH-].[Na+].C1COCC1>[F:2][C:3]1([F:9])[CH2:8][CH2:7][N:6]([C:20]2[N:19]=[C:18]3[C:17]4[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=4[C:11](=[O:10])[C:23]3=[N:22][C:21]=2[C:24]#[N:25])[CH2:5][CH2:4]1

참가 물질

5

반응물 2

HCID 2929299-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrileHCID 27583514,4-Difluoropiperidine hydrochloride

생성물 1

HCID 16065358HCID 16065358, 화합물수율 95%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매

실험 절차

4,4-Difluoropiperidine hydrochloride (249 mg, 1.58 mmol) was dissolved in 1N NaOH (5 ml) and extracted with CH2Cl2 (2×5 ml). Organic phase was dried over Na2SO4, filtered and evaporated. The residue was dissolved in THF (2 ml) and this solution was added to a solution of 1 (185 mg, 0.79 mmol) in THF (2 ml); the mixture was stirred at room temperature for 48 hours. The solvent was evaporated, the crude solid washed with EtOH and dried under vacuum, affording 8 (245 mg, 95%) as yellow-brown solid.

후처리

  1. extractionextracted with CH2Cl2 (2×5 ml)
  2. dry with materialOrganic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. dissolutionThe residue was dissolved in THF (2 ml)
  6. customThe solvent was evaporated
  7. washthe crude solid washed with EtOH
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-48e5c379424043b89874b39d371f86e2
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648076B2

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