Hydrochloric Acid → HCID 66835233, 화합물

HRID 2275276노트

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HRID 2275276 반응식
[CH3:1][C:2]1([CH3:31])[O:6][C@@H:5]([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[C:24](=[O:25])[C:23]4[C:22]5[C:17](=[CH:18][C:19]([C:26]#[N:27])=[CH:20][CH:21]=5)[NH:16][C:15]=4[C:14]([CH3:29])([CH3:28])[C:13]=3[CH:30]=2)[CH2:4][O:3]1.[Cl-].[NH4+].[N-:34]=[N+:35]=[N-:36].[Na+].Cl>CN(C=O)C>[CH3:1][C:2]1([CH3:31])[O:6][C@@H:5]([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[C:24](=[O:25])[C:23]4[C:22]5[C:17](=[CH:18][C:19]([C:26]6[N:34]=[N:35][NH:36][N:27]=6)=[CH:20][CH:21]=5)[NH:16][C:15]=4[C:14]([CH3:29])([CH3:28])[C:13]=3[CH:30]=2)[CH2:4][O:3]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium Azide2회HCID 66834868HCID 66834868, 화합물

생성물 1

HCID 66835233HCID 66835233, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

8-((S)-2,2-Dimethyl-[1,3]dioxolan-4-yl methoxy)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (20.0 mg, 0.048 mmol), ammonium chloride (1.28 mg, 0.024 mmol) and NaN3 (6.24 mg, 0.096 mmol) were dissolved in DMF, and the mixture was stirred at 120° C. for 14 hrs. NaN3 (6.24 mg, 0.096 mmol) was further added to the mixture, which was then stirred at 120° C. for 30 hrs. The reaction solution was added with 1 N aqueous solution of hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated brine and concentrated under reduced pressure. The resultant solid obtained after concentration was washed with hexane:ethyl acetate=1:1 to obtain 8-((S)-2,2-dimethyl-[1,3]dioxolan-4-yl methoxy)-6,6-dimethyl-3-(2H-tetrazol-5-yl)-5,6-dihydro-benzo[b]carbazol-11-one as a white solid.

후처리

  1. stirringwas then stirred at 120° C. for 30 hrs
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. concentrationconcentrated under reduced pressure
  5. customThe resultant solid obtained
  6. concentrationafter concentration
  7. washwas washed with hexane

출처 및 근거

ORD 기록
ord-fd3de1ce8cbb4cc3b70ceb3ef8ebe905
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126931B2

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