Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}piperidine hydrochloride

HRID 743328ノート

反応式

HRID 743328 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([O:32][CH3:33])[CH:27]=2)[CH2:9]1)=O)(C)(C)C.[ClH:34]>O1CCOCC1>[ClH:34].[CH3:33][O:32][C:28]1[CH:27]=[C:26]([CH2:25][CH2:24][CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:31]=[CH:30][CH:29]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 106473391-t-Butoxycarbonyl-3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}piperidine

生成物 1

HCID 574976463-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}piperidine hydrochloride収率 85%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

1.79 g of 1-t-butoxycarbonyl-3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}piperidine [prepared as described in step (a) above] were dissolved in 5 ml of dioxane and 5 ml of a 4N solution of hydrogen chloride in dioxane were added to the solution. The mixture was allowed to stand at room temperature for 2 hours, after which the solvent was removed by distillation under reduced pressure. The resulting residue was dissolved in 20 ml of ethyl acetate, and the solution was allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.31 g (yield 85%) of the title compound as needles, melting at 136°-137° C.

後処理

  1. customafter which the solvent was removed by distillation under reduced pressure
  2. dissolutionThe resulting residue was dissolved in 20 ml of ethyl acetate
  3. customto stand at room temperature
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-70a3b5a7eaa148fbbea063fc24065d75
出典データセット
uspto-grants-1996_09
特許番号
US05556864

反応ノート

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