Water → HCID 19743503, 화합물

HRID 2254033노트

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HRID 2254033 반응식
[K].[Cl:2][C:3]1[CH:19]=[CH:18][C:6]2[N:7]=[C:8]([O:10][C:11]3[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=3)[O:9][C:5]=2[CH:4]=1.[C:20]([CH:22]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=1[Cl:35])[C:23](=[O:27])[CH:24](Cl)[CH3:25])#[N:21].O>CN(C)C=O>[C:20]([CH:22]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=1[Cl:35])[C:23](=[O:27])[CH:24]([O:17][C:14]1[CH:13]=[CH:12][C:11]([O:10][C:8]2[O:9][C:5]3[CH:4]=[C:3]([Cl:2])[CH:19]=[CH:18][C:6]=3[N:7]=2)=[CH:16][CH:15]=1)[CH3:25])#[N:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 155475Phenol, 4-((6-chloro-2-benzoxazolyl)oxy)-HCID 5462222PotassiumHCID 197435991-Cyano-1-(2,4-dichlorophenyl)-3-chloro-2-butanone

생성물 1

HCID 19743503HCID 19743503, 화합물수율 46.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

2.70 Grams of a potassium salt of 4-(6-chloro-2-benzoxazolyloxy)phenol and 2.48 g of 1-cyano-1-(2,4-dichlorophenyl)-3-chloro-2-butanone were refluxed in 50 ml of N,N-dimethylformamide under heat at 100° C. for 4 hours. The reaction mixture was added to water, and after the mixture was subjected to extraction with chloroform, the extract was concentrated. The residue was separated and purified by column chromatography to give 2.05 g of a compound No. 176 which was a light yellow solid (melting point 93°-94° C.). The yield was 46.9%. The compound No. 176 was analyzed, and the results are shown in Tables 1 to 23.

후처리

  1. extractionafter the mixture was subjected to extraction with chloroform
  2. concentrationthe extract was concentrated
  3. customThe residue was separated
  4. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-3c209366620e4fa698b926cccc96231f
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05234894

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