Hydrochloric Acid → HCID 20161366, 화합물

HRID 247044노트

반응식

HRID 247044 반응식
[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

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 10340Sodium CarbonateHCID 20161359HCID 20161359, 화합물

생성물 1

HCID 20161366HCID 20161366, 화합물수율 72%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fcc75c7d0e2e42e9acc32b7e73f18a34
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705793

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