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HCID 18784149、化合物 → HCID 18784192、化合物

HRID 1108759
ノート
印刷プレビュー

反応式

HRID 1108759 の反応式
C([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=2)[CH2:10]1)C1C=CC=CC=1.[ClH:25].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:25].[CH3:24][O:23][C:17]1[CH:16]=[C:15]([CH:11]2[CH2:12][CH2:13][CH2:14][CH:9]([NH2:8])[CH2:10]2)[CH:20]=[CH:19][C:18]=1[O:21][CH3:22]
参加物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 18784149HCID 18784149、化合物HCID 21866389Hydrogen chloride-ethyl acetate

生成物 1

HCID 18784192HCID 18784192、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

N-Benzyl-N-[3-(3,4-dimethoxyphenyl)cyclohexyl]amine (3.16 g) was dissolved in ethyl acetate, 4 N HCl-ethyl acetate solution was added, and the mixture was stirred at room temperature for 30 minutes. After concentrating the solvent under reduced pressure, it was dissolved in acetic acid (100 ml), and 10% palladium-carbon (640 mg) was added thereto. After substituting the reaction vessel with hydrogen gas, hydrogen addition was effected for 3 hours at normal pressure, at 80° C. After the reaction, the catalyst was filtered off and the solvent was distilled off under reduced pressure to produce crude crystals which were then washed with diethyl ether to give 2.80 g of 3-(3,4-dimethoxyphenyl)cyclohexylamine hydrochloride (quantitative yield).

後処理

  1. concentrationAfter concentrating the solvent under reduced pressure, it
  2. dissolutionwas dissolved in acetic acid (100 ml)
  3. addition10% palladium-carbon (640 mg) was added
  4. additionwith hydrogen gas, hydrogen addition
  5. waitwas effected for 3 hours at normal pressure, at 80° C
  6. customAfter the reaction
  7. filtrationthe catalyst was filtered off
  8. distillationthe solvent was distilled off under reduced pressure
  9. customto produce crude crystals which
  10. washwere then washed with diethyl ether

出典と根拠

ORDレコード
ord-1d5bbbffbe2544ab8687a4c74f8464fb
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06069176

反応ノート

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