Sodium Hydroxide → DR 3438

HRID 1905085ノート

反応式

HRID 1905085 の反応式
[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])=[CH:10][O:11][C:6]=2[CH:5]=[C:4]([O:20][CH2:21][C:22]([O:24]CC)=[O:23])[CH:3]=1.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[C:7]2[C:8](=[O:19])[C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH3:18])=[CH:10][O:11][C:6]=2[CH:5]=[C:4]([O:20][CH2:21][C:22]([OH:24])=[O:23])[CH:3]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14254503ethyl {[5-chloro-3-(2-methylphenyl)-4-oxo-4H-1-benzopyran-7-yl]oxy}acetate

生成物 1

HCID 196673DR 3438収率 86%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 1.2 l of ethanol was suspended 132 g of ethyl {[5-chloro-3-(2-methylphenyl)-4-oxo-4H-1-benzopyran-7-yl]oxy}acetate, and 0.53 l of a 1N sodium hydroxide aqueous solution was slowly added dropwise to the suspension at room temperature, followed by stirring at room temperature for 3 hours. The insoluble material was removed by filtration, and the filtrate was acidified with hydrochloric acid while ice-cooling and stirring. The stirring was continued at room temperature overnight. The precipitated crystals were collected by filtration, washed with water, and dried to obtain 105 g of the entitled compound having a melting point of 191° to 192° C.

後処理

  1. additionwas slowly added dropwise to the suspension at room temperature
  2. customThe insoluble material was removed by filtration
  3. temperaturecooling
  4. stirringstirring
  5. waitThe stirring was continued at room temperature overnight
  6. filtrationThe precipitated crystals were collected by filtration
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-82ae7a74b9b64955ba6b7d3ae3080f79
出典データセット
uspto-grants-1989_06
特許番号
US04841076

反応ノート

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