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3-Oxocyclohexane-1-carboxylic acid → 9-(4-chlorobenzoyl)-6-methoxy-2,3,4,9-tetrahydro-1H-carbazole-2-carboxylic acid

HRID 527454
ノート
印刷プレビュー

反応式

HRID 527454 の反応式
O=[C:2]1[CH2:7][CH2:6][CH2:5][CH:4]([C:8]([OH:10])=[O:9])[CH2:3]1.Cl.[Cl:12][C:13]1[CH:30]=[CH:29][C:16]([C:17]([N:19]([C:21]2[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=2)N)=[O:18])=[CH:15][CH:14]=1>C(O)(=O)C>[Cl:12][C:13]1[CH:30]=[CH:29][C:16]([C:17]([N:19]2[C:2]3[CH2:3][CH:4]([C:8]([OH:10])=[O:9])[CH2:5][CH2:6][C:7]=3[C:22]3[C:21]2=[CH:26][CH:25]=[C:24]([O:27][CH3:28])[CH:23]=3)=[O:18])=[CH:15][CH:14]=1
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

4

反応物 2

HCID 27602523-Oxocyclohexane-1-carboxylic acidHCID 124352824-Chloro-benzoic Acid 1-(4-Methoxyphenyl)hydrazide Hydrochloride

生成物 1

HCID 218196899-(4-chlorobenzoyl)-6-methoxy-2,3,4,9-tetrahydro-1H-carbazole-2-carboxylic acid収率 82%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

3-Oxocyclohexanecarboxylic acid (27.2 mg, 0.19 mmol) was added to a stirred solution of 4-chloro-N-(4-methoxyphenyl)benzohydrazide hydrochloride (50 mg, 0.16 mmol) in acetic acid (0.5 mL), the mixture was heated at 80° C. under nitrogen for 3 h, then it was allowed to cool to ambient temperature and stirred overnight. Ice-water (2 mL) was poured into the cold reaction mixture and the formed precipitate was collected by filtration, carefully washed with water and dried in vacuo to yield the title compound (50 mg, 82%) as an off-white solid. C21H18ClNO4, Mr=383.82; 1H NMR (400 MHz, DMSO-d6) d: 1.79-1.87 (m, 1H), 2.11-2.14 (m, 1H), 2.57-2.75 (m, 5H), 6.73 (dd, J=2.8/9.0 Hz, 1H), 6.97 (d, J=2.8 Hz, 1H), 7.06 (d, J=9.2 Hz, 1H), 7.62-7.69 (m, 4H); LCMS (ESI) tR: 2.82 min (>99%, ELSD), m/z: 384.0 [M+1]+.

後処理

  1. temperatureto cool to ambient temperature
  2. filtrationthe formed precipitate was collected by filtration
  3. washcarefully washed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-1c6cb46038b849798104ee564b8046fa
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346803B2

反応ノート

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