Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride

HRID 743330ノート

反応式

HRID 743330 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1.[ClH:28].C(OCC)(=O)C>O1CCOCC1.CO>[ClH:28].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 100012501-Methyl-3-(2-(4-(3-methoxyphenyl)butyl)phenoxymethyl)piperidine

生成物 1

HCID 100012493-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride収率 83%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

2.10 g of 3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] were dissolved in 10 ml of dioxane, and 1.7 ml of a 4N solution of hydrogen chloride in dioxane was added to the solution, which was shaken and then concentrated by distillation under reduced pressure to give a solid. The solid was dissolved in a small amount of methanol, and then 50 ml of ethyl acetate were added to the solution. The resulting mixture was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.92 g (yield 83%) of the title compound as colorless needles, melting at 141°-142.5° C.

後処理

  1. concentrationconcentrated by distillation under reduced pressure
  2. customto give a solid
  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-b067ddbaddfa41c0b09e681211c1de31
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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