Water → [2-(4-Benzyloxyphenoxy)ethyl]dimethylamine

HRID 133771ノート

反応式

HRID 133771 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:17][N:18]([CH3:22])[CH2:19][CH2:20]Cl.[H-].[Na+].O>CN(C)C=O>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:20][CH2:19][N:18]([CH3:22])[CH3:17])=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 7638MonobenzoneHCID 24758Sodium hydrideHCID 11636816N,N-Dimethylaminoethyl chloride hydrochloride

生成物 1

HCID 59447665[2-(4-Benzyloxyphenoxy)ethyl]dimethylamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
90 °C

実験手順

4-(Benzyloxy)phenol (2.89 g, 0.01443 mol) in dimethylformamide (15 ml) and 2-(dimethylamino)ethyl chloride hydrochloride (2.32 g, 0.01611 mol) were added simultaneously in small portions to a 55-65% sodium hydride dispersion in mineral oil (0.033 mol) in dimethylformamide (5 ml) at 0° C. Then the mixture was allowed to warm to 90° C., and stirring was continued for 1.5 h. The cooled mixture was poured into water. The resultant mixture was extracted with toluene. The combined extracts were washed with 2.5 M NaOH and water and dried over Na2SO4. Toluene was evaporated and the residual product was used as such in the next step.

後処理

  1. extractionThe resultant mixture was extracted with toluene
  2. washThe combined extracts were washed with 2.5 M NaOH and water
  3. dry with materialdried over Na2SO4
  4. customToluene was evaporated

出典と根拠

ORDレコード
ord-4ca4431bf066407e882feaaa0ee348f4
出典データセット
uspto-grants-2008_06
特許番号
US07390923B2

反応ノート

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