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Hydrochloric Acid → HCID 14674164、化合物

HRID 1614210
ノート
印刷プレビュー

反応式

HRID 1614210 の反応式
Br[CH2:2][C:3]([C:5]1[CH:14]=[CH:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=1)=[O:4].[ClH:15].[N+:16]([C:19]1[CH:20]=[C:21]([CH:29]=[CH:30][CH:31]=1)[O:22][CH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1)([O-:18])=[O:17].C(N(CC)CC)C.Cl>C(O)C>[ClH:15].[N+:16]([C:19]1[CH:20]=[C:21]([CH:29]=[CH:30][CH:31]=1)[O:22][CH:23]1[CH2:24][CH2:25][N:26]([CH2:2][C:3]([C:5]2[CH:14]=[CH:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH:6]=2)=[O:4])[CH2:27][CH2:28]1)([O-:18])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 691792-Bromo-2'-acetonaphthoneHCID 224033414-(3-Nitrophenoxy)piperidine hydrochloride

生成物 1

HCID 14674164HCID 14674164、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.63 g of 2-bromo-2'-acetonaphthone, 0.65 g of 4-(m-nitrophenoxy)piperidine hydrochloride, and 1 g of triethylamine were added to 100 ml of ethanol. The mixture was refluxed for 30 min. The solvent was distilled off, and dichloromethane was added to the residue. The mixture was washed with water and dried. The dichloromethane was distilled off, and the residue was purified by column chromatography (silica gel) to prepare an oleaginous intended compound. The compound was converted into a hydrochloride by an ordinary method and then recrystallized to prepare 0.15 g of an intended hydrochloride.

後処理

  1. temperatureThe mixture was refluxed for 30 min
  2. distillationThe solvent was distilled off
  3. additiondichloromethane was added to the residue
  4. washThe mixture was washed with water
  5. customdried
  6. distillationThe dichloromethane was distilled off
  7. customthe residue was purified by column chromatography (silica gel)
  8. customto prepare an oleaginous intended compound
  9. customrecrystallized
  10. customto prepare 0.15 g of an intended hydrochloride

出典と根拠

ORDレコード
ord-0036256189be44d4a9a75fe69f54fd79
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05196439

反応ノート

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