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Isoniazid → HCID 20450003, 화합물

HRID 358054
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HRID 358054 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=S)[CH2:9][CH:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[C:6]=2[CH:20]=1.[C:21]([NH:29][NH2:30])(=O)[C:22]1[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=1>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:21]([C:22]4[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=4)=[N:29][N:30]=[C:10]3[CH2:9][CH:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[F:19])[C:6]=2[CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3767IsoniazidHCID 20449980HCID 20449980, 화합물

생성물 1

HCID 20450003HCID 20450003, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

6 g of 7-chloro-5-(2-fluorophenyl)-1,3-dihydro-2H-1-benzazepine-2-thione and 27 g of isonicotinic acid hydrazide are dissolved together in 360 ml of n-butanol and heated to boiling under reflux for 24 hours. After evaporation of the resulting solution in vacuo, the residue is partitioned between toluene and water. The toluene phase is concentrated to about 100 ml. The precipitated crystals are filtered off and recrystallized from benzene. There is obtained 8-chloro-6-(2-fluorophenyl)-1-(4-pyridyl)-4H-s-triazolo[4,3-a][1]benzazepine of melting point 198°-200°.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 24 hours
  3. customAfter evaporation of the resulting solution in vacuo
  4. customthe residue is partitioned between toluene and water
  5. concentrationThe toluene phase is concentrated to about 100 ml
  6. filtrationThe precipitated crystals are filtered off
  7. customrecrystallized from benzene

출처 및 근거

ORD 기록
ord-aac6158a99d74c82ae445579ce8c2cc1
출처 데이터셋
uspto-grants-1984_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04464300

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