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3-(2-Chloroethyl)-1,3-oxazolidin-2-one → HCID 13136716、化合物

HRID 2164756
ノート
印刷プレビュー

反応式

HRID 2164756 の反応式
[Na+].[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[C:15](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:16]([O-:18])=[O:17])=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.Cl[CH2:24][CH2:25][N:26]1[CH2:30][CH2:29][O:28][C:27]1=[O:31]>CN(C)C=O>[O:31]=[C:27]1[N:26]([CH2:25][CH2:24][O:17][C:16](=[O:18])[C:15]2[C:14](=[CH:22][CH:21]=[CH:20][CH:19]=2)[NH:13][C:7]2[C:6]3[C:11](=[CH:12][C:3]([Cl:2])=[CH:4][CH:5]=3)[N:10]=[CH:9][CH:8]=2)[CH2:30][CH2:29][O:28]1
参加物反応条件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 756333-(2-Chloroethyl)-1,3-oxazolidin-2-oneHCID 23701501HCID 23701501、化合物

生成物 1

HCID 13136716HCID 13136716、化合物収率 68.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A mixture comprising 12.8 g of N-(7-chloro-4-quinolyl)-anthranilic acid sodium salt, 6.64 g of 90% 3-(β-chloroethyl)-oxazolidine-2-one and 80 ml of dimethylformamide was heated under stirring at 120° C. for five hours. Upon completion of the reaction, the mixture was cooled, filtered, and the solvent eliminated in vacuo. To the residue, 80 ml of ether were added and the solid thus obtained was collected on filter and purified by chromatography on a silica gel column using ethyl acetate as eluent. The desired product was crystallized from isopropanol to give 11.2 g of N-(7-chloro-4-quinolyl)-anthranilic acid β-(2-oxo-3-oxazolidinyl)-ethyl ester, melting at 122°-124° C.

後処理

  1. temperaturewas heated
  2. customUpon completion of the reaction
  3. temperaturethe mixture was cooled
  4. filtrationfiltered
  5. additionTo the residue, 80 ml of ether were added
  6. customthe solid thus obtained
  7. customwas collected
  8. filtrationon filter
  9. custompurified by chromatography on a silica gel column
  10. customThe desired product was crystallized from isopropanol

出典と根拠

ORDレコード
ord-c8f714e3fda8479698eb1d37a52888f0
出典データセット
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04507308

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート