3-Hydroxybenzaldehyde → 3-[(3-Methylpiperidin-1-yl)methyl]phenol

HRID 4648

反応式

HRID 4648 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.[CH3:10][CH:11]1[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1.C(O)=O.N>O>[CH3:10][CH:11]1[CH2:16][CH2:15][CH2:14][N:13]([CH2:5][C:4]2[CH:3]=[C:2]([OH:1])[CH:9]=[CH:8][CH:7]=2)[CH2:12]1

参加物

6

反応物 4

HCID 1013-HydroxybenzaldehydeHCID 222AmmoniaHCID 284Formic AcidHCID 790813-Methylpiperidine

生成物 1

HCID 133646663-[(3-Methylpiperidin-1-yl)methyl]phenol

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

24.4 g (0.2 mol) of 3-hydroxybenzaldehyde are mixed with 40 ml (about 0.4 mol) of 3-methylpiperidine and 20 ml (about 0.52 mol) of 100% formic acid with cooling and then stirred for 2 hours at 120° C. When the reaction mixture has cooled to room temperature, it is poured into water and rendered alkaline with ammonia, and the precipitated solid is filtered off and recrystallised from ethanol.

後処理

  1. temperaturewith cooling
  2. temperatureWhen the reaction mixture has cooled to room temperature
  3. filtrationthe precipitated solid is filtered off
  4. customrecrystallised from ethanol

出典と根拠

ORDレコード
ord-e9c53b21b5524c4296badbb52530d5b3
出典データセット
uspto-grants-1988_02
特許番号
US04727081

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