4-Hydroxybenzaldehyde → 4-(3-Dibutylamino-propoxy)-benzaldehyde

HRID 1048911

反応式

HRID 1048911 の反応式
Cl.[CH2:2]([N:6]([CH2:11][CH2:12][CH2:13]Cl)[CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][CH2:4][CH3:5].[OH:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=[O:21])=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].CCC(C)=O>O>[CH2:2]([N:6]([CH2:7][CH2:8][CH2:9][CH3:10])[CH2:11][CH2:12][CH2:13][O:15][C:16]1[CH:23]=[CH:22][C:19]([CH:20]=[O:21])=[CH:18][CH:17]=1)[CH2:3][CH2:4][CH3:5]

参加物

6

反応物 4

HCID 1264-HydroxybenzaldehydeHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 225950531-Dibutylamino-3-chloropropane hydrochloride

生成物 1

HCID 141464004-(3-Dibutylamino-propoxy)-benzaldehyde収率 90.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

9.69 g of dibutylamino propylchloride HCl salt (IV) (0.04 mol, 1 eq), 5 g of 4-hydroxybenzaldehyde (III) (0.04 mol, 1 eq), 17 g of potassium carbonate (0.12 mol, 3 eq) and 30 mL of MEK are added to the reaction flask. The suspension is heated to 80° C. and it is stirred for 10 hours at this temperature. Then the mixture is cooled to room temperature, 40 mL of water is added and the brown solution is stirred for 30 min. After phase separation the organic phase is washed with 15 mL of water and the solvent is evaporated to obtain 10.6 g of compound (V) as a yellowish-brown solid (89%).

後処理

  1. temperatureThen the mixture is cooled to room temperature
  2. stirringthe brown solution is stirred for 30 min
  3. customAfter phase separation the organic phase
  4. washis washed with 15 mL of water
  5. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-33d6c86450a443948090e15be20b79b6
出典データセット
uspto-grants-2016_07
特許番号
US09382223B2

関連ノート

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