ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Formaldehyde → 2-Cyclohexen-1-one, 5,5-dimethyl-3-(2-chlorophenylamino)-2-piperidinomethyl-, monohydrochloride

HRID 918144
ノート
印刷プレビュー

反応式

HRID 918144 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[NH:4][C:5]1[CH2:10][C:9]([CH3:12])([CH3:11])[CH2:8][C:7](=[O:13])[CH:6]=1.[CH2:18]=O.Cl.[NH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1>CO.C(O)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[NH:4][C:5]1[CH2:10][C:9]([CH3:12])([CH3:11])[CH2:8][C:7](=[O:13])[C:6]=1[CH2:18][N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1
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 3

HCID 712FormaldehydeHCID 2723721Piperidine, hydrochloride (1:1)HCID 13002203HCID 13002203、化合物

生成物 1

HCID 30399422-Cyclohexen-1-one, 5,5-dimethyl-3-(2-chlorophenylamino)-2-piperidinomethyl-, monohydrochloride

試薬・触媒・溶媒 2

HCID 176Acetic Acid触媒HCID 887Methanol
溶媒

実験手順

12.5 Parts of 3-(2-chloroanilino)-5,5-dimethyl-2-cyclohexen-1-one is dissolved in 30 volume parts of methanol under warming and, then, to the resulting solution are added 4.5 parts of a 37 weight % aqueous solution of formaldehyde, 6.05 parts of piperidine hydrochloride and 2 drops of glacial acetic acid. The whole mixture is allowed to stand at room temperature for 1 hour, whereupon a yellow, clear solution is obtained. The methanol is distilled off under reduced pressure, and a small amount of isopropyl ether is added to the resulting residue, followed by cooling, whereupon colorless crystals separate. The crystals are collected by filtration and recrystallized from acetone. The procedure yields colorless prisms of 3-(2-chloroanilino)-5,5-dimethyl-2-piperidinomethyl-2-cyclohexen-1-one hydrochloride. Melting point: 105°-106°C. Elementary analysis: C20H28N2OCl2.1/2H2O Calcd. C, 61.21; H, 7.45; N, 7.14 Found C, 60.91; H, 7.60; N, 7.25.

後処理

  1. temperatureunder warming
  2. customwhereupon a yellow, clear solution is obtained
  3. distillationThe methanol is distilled off under reduced pressure
  4. additiona small amount of isopropyl ether is added to the resulting residue
  5. temperatureby cooling, whereupon colorless crystals
  6. customseparate
  7. filtrationThe crystals are collected by filtration
  8. customrecrystallized from acetone

出典と根拠

ORDレコード
ord-2eccda436fb44c31b2d6cb9ee051ae21
出典データセット
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03969409

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート