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N-bromobutanimide → 4-bromo-2,2-dimethyl-5-(thiazol-4-yl)furan-3(2H)-one

HRID 1425903
ノート
印刷プレビュー

反応式

HRID 1425903 の反応式
[CH3:1][C:2]1([CH3:13])[C:6](=[O:7])[CH:5]=[C:4]([C:8]2[N:9]=[CH:10][S:11][CH:12]=2)[O:3]1.C1C(=O)N([Br:21])C(=O)C1>C(Cl)(Cl)Cl.C(Cl)Cl>[Br:21][C:5]1[C:6](=[O:7])[C:2]([CH3:13])([CH3:1])[O:3][C:4]=1[C:8]1[N:9]=[CH:10][S:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 593548052,2-dimethyl-5-(thiazol-4-yl)furan-3(2H)-one

生成物 1

HCID 593548524-bromo-2,2-dimethyl-5-(thiazol-4-yl)furan-3(2H)-one収率 71%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 2,2-dimethyl-5-(thiazol-4-yl) furan-3(2H)-one (90 mg, 0.46 mmol) in CHCl3 (1.8 mL) was added NBS (0.12 g, 0.69 mmol) portionwise at RT and the reaction mixture was stirred for 1 h. The reaction mixture was diluted with DCM (10 mL), washed with water (5 mL), brine (10 mL), dried over Na2SO4, filtered and then concentrated in vacuo to obtain the crude product. The crude material was purified via silica gel column chromatography to afford 4-bromo-2,2-dimethyl-5-(thiazol-4-yl) furan-3(2H)-one (40 mg, 71%) as an off white solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. washwashed with water (5 mL), brine (10 mL)
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto obtain the crude product
  6. customThe crude material was purified via silica gel column chromatography

出典と根拠

ORDレコード
ord-a54606957fec48c5b742222194b645df
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933074B2

反応ノート

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