Sodium Hydroxide → DR 3438

HRID 1905085노트

반응식

HRID 1905085 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 196673DR 3438수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-82ae7a74b9b64955ba6b7d3ae3080f79
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04841076

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