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

HRID 240309

反応式

HRID 240309 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 16065358HCID 16065358、化合物収率 95%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-48e5c379424043b89874b39d371f86e2
出典データセット
uspto-grants-2014_02
特許番号
US08648076B2

関連ノート

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