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Isopropanol → HCID 178459484, 화합물

HRID 428427
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HRID 428427 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
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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-f09f6840a9a2425b820a8476986ec3bd
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06313290B1

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