Hydrochloric Acid → HCID 20161366、化合物

HRID 247044ノート

反応式

HRID 247044 の反応式
[NH2:1][C:2]1[C:11]2[C:10](=[O:12])[N:9]([CH2:13][C:14]#[CH:15])[CH2:8][CH2:7][C:6]=2[N:5]=[C:4]2[N:16](C=C)[N:17]=[CH:18][C:3]=12.Cl.O.C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C>[NH2:1][C:2]1[C:11]2[C:10](=[O:12])[N:9]([CH2:13][C:14]#[CH:15])[CH2:8][CH2:7][C:6]=2[N:5]=[C:4]2[NH:16][N:17]=[CH:18][C:3]=12

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 10340Sodium CarbonateHCID 20161359HCID 20161359、化合物

生成物 1

HCID 20161366HCID 20161366、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a mechanically stirred solution of 4-amino-7,8-dihydro-6-(prop-2-ynyl)-1-vinyl-1H-pyrazolo[3,4-b][1,6]napthyridin-5(6H)-one (1.91 g.) in dry acetonitrile (35 ml.) under a nitrogen atmosphere was added freshly prepared 6N aqueous HCl (11.65 ml.) at room temperature. The resulting suspension was heated under reflux for three hours, followed by cooling to room temperature and addition of water. The reaction mixture was made basic with aqueous saturated sodium carbonate and extracted with EtOAc. The organic phase was washed with brine, dried over magnesium sulfate, filtered through diatomaceous earth and concentrated to give 4-amino-7,8-dihydro-6-(prop-2-ynyl)-1H-pyrazolo[3,4-b][1,6]napthyridin-5(6H)-one as a white solid (1.24 g.) (72% yield) which was used without further purification.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureunder reflux for three hours
  3. extractionextracted with EtOAc
  4. washThe organic phase was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered through diatomaceous earth
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-fcc75c7d0e2e42e9acc32b7e73f18a34
出典データセット
uspto-grants-1987_11
特許番号
US04705793

反応ノート

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