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2-(Dimethylamino)ethanol → HCID 53923166、化合物

HRID 2225707
ノート
印刷プレビュー

反応式

HRID 2225707 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[O:11][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21](=[O:25])[C:22]([OH:24])=[O:23])=[CH:17][CH:16]=1.[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29]O>ClCCl>[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][O:23][C:22](=[O:24])[C:21](=[O:25])[C:18]1[CH:19]=[CH:20][C:15]([O:14][CH2:13][CH2:12][O:11][C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=3)[CH:1]=2)=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 79022-(Dimethylamino)ethanolHCID 19004267HCID 19004267、化合物

生成物 1

HCID 53923166HCID 53923166、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The acid chloride, prepared from 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alphaoxobenzeneacetic acid (0.5 g) as described in Example 6, was dissolved in dichloromethane (10 mL) and added dropwise to a stirred, cold (<-50° C.) mixture of 2-(dimethylamino)ethanol (0.178 g) in dichloromethane (10 mL). The cooling bath was removed and the mixture stirred for 1 hour at room temperature. The mixture was diluted with dichloromethane and washed once with saturated aqueous sodium bicarbonate, once with water, and the organic solution was dried (Na2SO4), filtered, and evaporated to give crude product. Crystallization from diethyl ether-hexane provided pure 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-(dimethylamino)ethyl ester as a colorless solid, mp 93°-94° C.

後処理

  1. customThe cooling bath was removed
  2. additionThe mixture was diluted with dichloromethane
  3. washwashed once with saturated aqueous sodium bicarbonate, once with water
  4. dry with materialthe organic solution was dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give crude product
  8. customCrystallization from diethyl ether-hexane provided pure 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-(dimethylamino)ethyl ester as a colorless solid, mp 93°-94° C.

出典と根拠

ORDレコード
ord-d3b91e4f16c441a4aac0ff0ca67f80f2
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05344843

反応ノート

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