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Ammonium Chloride → HCID 66834635、化合物

HRID 2275194
ノート
印刷プレビュー

反応式

HRID 2275194 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:16]=[CH:17][C:18]3[C:30](=[O:31])[C:29]4[C:28]5[C:23](=[CH:24][CH:25]=[C:26]([N+:32]([O-])=O)[CH:27]=5)[NH:22][C:21]=4[C:20]([CH3:36])([CH3:35])[C:19]=3[CH:37]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+]>[Fe].C(O)C>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:16]=[CH:17][C:18]3[C:30](=[O:31])[C:29]4[C:28]5[C:23](=[CH:24][CH:25]=[C:26]([NH2:32])[CH:27]=5)[NH:22][C:21]=4[C:20]([CH3:36])([CH3:35])[C:19]=3[CH:37]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 66834037HCID 66834037、化合物

生成物 1

HCID 66834635HCID 66834635、化合物収率 118.5%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

To the ethanol (8 ml) suspension of 4-(6,6-dimethyl-2-nitro-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-8-yl oxy)-piperidine-1-carboxylic acid tert-butyl ester (Compound P4, 103 mg, 0.204 mmol), iron powder (228 mg, 20 eq.), ammonium chloride (109 mg, 10 eq.), and distilled water (4 ml) were added and the mixture was stirred at 90° C. for 30 min. Upon the completion of the reaction, insoluble matters were filtered off, and the filtrate was extracted with ethyl acetate. The organic layer was washed with brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (115 mg, 57%).

後処理

  1. distillationdistilled water (4 ml)
  2. additionwere added
  3. customUpon the completion of the reaction, insoluble matters
  4. filtrationwere filtered off
  5. extractionthe filtrate was extracted with ethyl acetate
  6. washThe organic layer was washed with brine
  7. dry with materialdried over sodium sulfate
  8. customThe drying agent was removed by filtration
  9. customthe residues obtained
  10. concentrationafter concentration under reduced pressure
  11. customwere purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-2b4a0369f25740ce89d3f8a1f6c0b932
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09126931B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート