Boron tribromide → HCID 57777377, 화합물

HRID 660825노트

반응식

HRID 660825 반응식
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

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 68838631HCID 68838631, 화합물

생성물 1

HCID 57777377HCID 57777377, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f6f8faa5491345ae9425ad18de3add47
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084448B2

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