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Isopropanol → HCID 178459484, 화합물

HRID 1954742
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HRID 1954742 반응식
[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6](=[O:20])[C:7]3[C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[N:13][NH:12][C:8]=3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.[CH3:23]C(O)C>Cl>[Cl:1][C:2]1[CH:22]=[CH:21][C:5]2[C:6](=[O:20])[C:7]3[C:14]([C:15]([O:17][CH:18]([CH3:23])[CH3:19])=[O:16])=[N:13][NH:12][C:8]=3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3776IsopropanolHCID 1784704817-Chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10-(1H,9H)dione

생성물 1

HCID 178459484HCID 178459484, 화합물수율 48%

시약·촉매·용매 1

HCID 313Hydrochloric Acid촉매

실험 절차

A solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (500 mg, 1.56 mmol), 2-propanol (60 mL), and concentrated hydrochloric acid (3 drops) was subjected to three cycles of partial solvent removal by slow distillation (over 6 hours) followed by overnight reflux. After the third cycle, solvent was removed by rotary evaporation and the crude product was purified by flash chromatography eluting with dichloromethane:2-propanol (95:5-85:15) to yield the title compound as a white solid (256 mg, 48%, m.p. 291° C). Alternatively, the title compound can be prepared as described in Example 18 shown hereinbelow in Table 1.

후처리

  1. temperaturereflux
  2. customAfter the third cycle, solvent was removed by rotary evaporation
  3. customthe crude product was purified by flash chromatography
  4. washeluting with dichloromethane:2-propanol (95:5-85:15)

출처 및 근거

ORD 기록
ord-0bea96bc1f4340cb9dd29795c317afc6
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06124281

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