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Hydrochloric Acid → N-(5-bromo-4-methylthiazol-2-yl)-2,6-difluorobenzamide

HRID 1255115
ノート
印刷プレビュー

反応式

HRID 1255115 の反応式
[NH2:1][C:2]1[S:3][C:4]([Br:11])=[C:5]([C:7](F)(F)F)[N:6]=1.[F:12][C:13]1[CH:21]=[CH:20][CH:19]=[C:18]([F:22])[C:14]=1[C:15](Cl)=[O:16].Cl>C1COCC1.N1C=CC=CC=1>[Br:11][C:4]1[S:3][C:2]([NH:1][C:15](=[O:16])[C:14]2[C:13]([F:12])=[CH:21][CH:20]=[CH:19][C:18]=2[F:22])=[N:6][C:5]=1[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 874382,6-Difluorobenzoyl chlorideHCID 157107015-Bromo-4-(trifluoromethyl)-1,3-thiazol-2-amine

生成物 1

HCID 59004504N-(5-bromo-4-methylthiazol-2-yl)-2,6-difluorobenzamide収率 83%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028
Tetrahydrofuran
溶媒

実験手順

2-Amino-5-bromo-4-trifluoromethylthiazole (0.8 g) was dissolved in 3 mL of 1:1 mixture of THF and pyridine. 2,6-difluorobenzoylchloride (0.6 g) was added at room temperature with stirring. The mixture was stirred for 3 hours at room temperature. The mixture was poured into ice water and acidified with aqueous hydrochloric acid then extracted with chloroform. The organic layer was dried over Na2SO4 and the solvent was removed under reduced pressure. Flash chromatography on silica gel gave the title compound as a white solid. Yield 83%.

後処理

  1. stirringThe mixture was stirred for 3 hours at room temperature
  2. extractionthen extracted with chloroform
  3. dry with materialThe organic layer was dried over Na2SO4
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-4b25ee29242644d2a6e5c548bebbf70c
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08455658B2

反応ノート

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