N-bromobutanimide → HCID 67212702, 화합물

HRID 1671346노트

반응식

HRID 1671346 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:10]2[N:17]=[C:16]([CH3:18])[CH:15]=[C:11]2[O:12][C:13]=1[CH3:14].C1C(=O)N([Br:26])C(=O)C1>CN(C=O)C>[Br:26][C:15]1[C:16]([CH3:18])=[N:17][N:10]2[C:9]([C:3]3[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=3[Cl:1])=[C:13]([CH3:14])[O:12][C:11]=12

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 591860073-(2,4-Dichloro-phenyl)-2,6-dimethyl-pyrazolo[5,1-b]oxazole

생성물 1

HCID 67212702HCID 67212702, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 3-(2,4-dichloro-phenyl)-2,6-dimethyl-pyrazolo[5,1-b]oxazole (Intermediate HE) (0.755 g, 2.69 mmol) in DMF (10 ml) is added NBS (0.502 g, 2.82 mmol). The reaction is stirred at RT for 30 mins and then partitioned between Na2CO3 and EtOAc. The mixture is extracted with EtOAc (×2) and the combined organic phases are dried over Na2SO4, filtered and evaporated to dryness under reduced pressure. This resulting solid is recrystallised from hot EtOAc/iso-hexane to yield the title compound. MS: m/z 360.99 [M+H]+

후처리

  1. custompartitioned between Na2CO3 and EtOAc
  2. extractionThe mixture is extracted with EtOAc (×2)
  3. dry with materialthe combined organic phases are dried over Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure
  6. customThis resulting solid is recrystallised from hot EtOAc/iso-hexane

출처 및 근거

ORD 기록
ord-afff5bd28cc7413784a6fd549866e190
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07994203B2

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