Boron tribromide → HCID 67081467、化合物

HRID 1188746ノート

反応式

HRID 1188746 の反応式
B(Br)(Br)Br.[I:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[S:13][C:14]3[CH:20]=[C:19]([O:21]C)[CH:18]=[CH:17][C:15]=3[N:16]=2)=[CH:8][CH:7]=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[I:5][C:6]1[CH:7]=[CH:8][C:9]([C:12]2[S:13][C:14]3[CH:20]=[C:19]([OH:21])[CH:18]=[CH:17][C:15]=3[N:16]=2)=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 67081740HCID 67081740、化合物

生成物 1

HCID 67081467HCID 67081467、化合物収率 55.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Boron tribromide (1 M in CH2Cl2, 6 mL) was added to an anhydrous CH2Cl2 (20 mL) solution of 4 (550 mg, 1.5 mmol). After stirring at room temperature for 24 h, the reaction mixture was quenched with ice water (10 mL) and neutralized with solid NaHCO3 (1.51 g, 18.0 mmol). The mixture was diluted with pH 7 buffer solution (Fisher, 20 mL) and extracted with dichloromethane-methanol (4:1, 3×100 mL). The extracts were combined, dried with anhydrous Na2SO4, and evaporated. The residue was treated with CH2Cl2/MeOH, to give pure 2-(4-iodophenyl)-1,3-benzothiazol-6-ol (5) as a white solid (295 mg, 55.8%).

後処理

  1. customthe reaction mixture was quenched with ice water (10 mL)
  2. extractionextracted with dichloromethane-methanol (4:1, 3×100 mL)
  3. dry with materialdried with anhydrous Na2SO4
  4. customevaporated
  5. additionThe residue was treated with CH2Cl2/MeOH

出典と根拠

ORDレコード
ord-3e2288c7e9294c48b27b8db8561f7ea9
出典データセット
uspto-grants-2014_03
特許番号
US08674101B2

反応ノート

読み込み中…