Hydrochloric Acid → HCID 66835233、化合物

HRID 61898ノート

反応式

HRID 61898 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium Azide2 回HCID 66834868HCID 66834868、化合物

生成物 1

HCID 66835233HCID 66835233、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a97a80a548b34a94b5e650858e3d0c8e
出典データセット
uspto-grants-2016_09
特許番号
US09440922B2

反応ノート

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