Boron tribromide → HCID 57777377、化合物

HRID 660825ノート

反応式

HRID 660825 の反応式
C([O:8][C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[N:16]1[S:20](=[O:22])(=[O:21])[NH:19][C:18](=[O:23])[CH2:17]1)C1C=CC=CC=1.B(Br)(Br)Br>C(Cl)Cl>[Cl:15][C:13]1[CH:12]=[CH:11][C:10]([N:16]2[S:20](=[O:22])(=[O:21])[NH:19][C:18](=[O:23])[CH2:17]2)=[C:9]([OH:8])[CH:14]=1

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 68838631HCID 68838631、化合物

生成物 1

HCID 57777377HCID 57777377、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 5-(2-benzyloxy-4-chlorophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (388 mg, 1.1 mmol) in methylene chloride (10 mL) at 0° C. is added dropwise BBr3 (1.65 mL of 1.0M in methylene chloride, 1.65 mmol) and the mixture is stirred at 0° C. for 30 min. Ice is added and the organic phase is washed with 1N HCl. The aqueous phase is washed with methylene chloride and the combined organic layers are dried over sodium sulfate. The solvent is removed under reduced pressure and the residue is purified by preparative HPLC to give the title compound as a white solid: (M−1)−=261.

後処理

  1. additionIce is added
  2. washthe organic phase is washed with 1N HCl
  3. washThe aqueous phase is washed with methylene chloride
  4. dry with materialthe combined organic layers are dried over sodium sulfate
  5. customThe solvent is removed under reduced pressure
  6. customthe residue is purified by preparative HPLC

出典と根拠

ORDレコード
ord-f6f8faa5491345ae9425ad18de3add47
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

反応ノート

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