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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
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Triethylene Glycol → HCID 53897125、化合物

HRID 2225706
ノート
印刷プレビュー

反応式

HRID 2225706 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.[CH2:26]([OH:35])[CH2:27][O:28][CH2:29][CH2:30][O:31][CH2:32][CH2:33]O>ClCCl>[OH:35][CH2:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH2:32][CH2:33][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 8172Triethylene GlycolHCID 19004267HCID 19004267、化合物

生成物 1

HCID 53897125HCID 53897125、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]-alpha-oxobenzene-acetic 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 triethylene glycol (0.9 g) in dichloro-methane (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. The material was purified by HPLC (dichloro-methane-ethyl acetate; 2:1) to provide, after crystallization from ethyl acetate-hexane, 0.36 g of 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-[2-(2-hydroxyethoxy)ethoxy]ethyl ester as a colorless solid, mp 70°-71° 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. customThe material was purified by HPLC (dichloro-methane-ethyl acetate; 2:1)
  9. customto provide
  10. customafter crystallization from ethyl acetate-hexane, 0.36 g of 4-[[2-(2-naphthalenyloxy)ethyl]oxy]-alpha-oxobenzeneacetic acid 2-[2-(2-hydroxyethoxy)ethoxy]ethyl ester as a colorless solid, mp 70°-71° C.

出典と根拠

ORDレコード
ord-093eea8ce8564cf3ada812be7e90d553
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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