Benzyloxyamine hydrochloride → HCID 178419047, 화합물

HRID 496685

반응식

HRID 496685 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]=[C:6](SC)[C:5]12[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.Cl.[CH2:19]([O:26][NH2:27])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CO>[CH2:19]([O:26][N:27]=[C:6]1[C:5]2([CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)[C:4]2[C:8](=[CH:9][CH:10]=[C:2]([Br:1])[CH:3]=2)[NH:7]1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

참가 물질

4

반응물 2

HCID 102312Benzyloxyamine hydrochlorideHCID 219862665'-Bromo-2'-(methylthio)spiro[cyclohexane-1,3'-[3H]indole]

생성물 1

HCID 178419047HCID 178419047, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
45 °C

실험 절차

5′-Bromo-2′-(methylthio)spiro[cyclohexane-1,3′-[3H ]indole] (9.0 g, 28.98 mmol) and O-benzylhydroxylamine hydrochloride (13.8 g, 86.9 .mmol) were combined in methanol (150 mL) and heated to 45° C. for 6 hours. Methanol was evaporated in vacuo. Ethyl acetate was added to the residue and this mixture was washed with ammonium chloride solution. Ethyl acetate was dried over magnesium sulfate, ethyl acetate collected evaporated in vacuo and the residue was flash chromatographed on alumina 90 (9:1Hexane/EtOAc) to the desired product (6.5 g, 60%).

후처리

  1. customMethanol was evaporated in vacuo
  2. additionEthyl acetate was added to the residue
  3. washthis mixture was washed with ammonium chloride solution
  4. dry with materialEthyl acetate was dried over magnesium sulfate, ethyl acetate
  5. customcollected
  6. customevaporated in vacuo
  7. customchromatographed on alumina 90 (9:1Hexane/EtOAc) to the desired product (6.5 g, 60%)

출처 및 근거

ORD 기록
ord-cb1327f5964c4c7fb782c4a801d50834
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06946454B2

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