N-bromobutanimide → HCID 67212702、化合物

HRID 1671346ノート

反応式

HRID 1671346 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 67212702HCID 67212702、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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]+

後処理

  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

出典と根拠

ORDレコード
ord-afff5bd28cc7413784a6fd549866e190
出典データセット
uspto-grants-2011_08
特許番号
US07994203B2

反応ノート

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