Hydrochloric Acid → HCID 135554955, 화합물

HRID 1379024노트

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HRID 1379024 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:11]3[N:12]=[N:13][CH:14]=[CH:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1.C([BH3-])#N.[Na+].Cl>CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:11]3[NH:12][NH:13][CH2:14][CH2:15][N:10]3[N:9]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 5003444Sodium cyanoborohydrideHCID 22909019HCID 22909019, 화합물

생성물 1

HCID 135554955HCID 135554955, 화합물수율 92.4%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
80 °C

실험 절차

To a suspension of 7-(4-fluorophenyl)-8-(pyridin-4-yl)pyrazolo[5,1-c][1,2,4]triazine (2.2 g) in methanol (20 ml) was added sodium cyanoborohydride (480 mg). The pH of the mixture was maintained at 3 to 4 for 2 hours with 1N hydrochloric acid. The procedure was repeated three additional times to completely finish the reduction. Then, the mixture was concentrated in vacuo and the residue was dissolved in 2N hydrochloric acid. The mixture was stirred at 80° C. for 30 minutes and cooled. The solution was neutralized with an aqueous saturated sodium bicarbonate solution. The separated solid was collected, washed with water and methanol and dried to give 7-(4-fluorophenyl)-8-(pyridin-4-yl)-1,2,3,4-tetrahydropyrazolo[5,1-c][1,2,4]triazine (2.06 g).

후처리

  1. concentrationThen, the mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in 2N hydrochloric acid
  3. temperaturecooled
  4. customThe separated solid was collected
  5. washwashed with water and methanol
  6. customdried

출처 및 근거

ORD 기록
ord-f2d638b3eeef4d48b17ef22c64f2366c
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05670503

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