Benzyloxyamine hydrochloride → HCID 178419047、化合物

HRID 496685

反応式

HRID 496685 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178419047HCID 178419047、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
45 °C

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-cb1327f5964c4c7fb782c4a801d50834
出典データセット
uspto-grants-2005_09
特許番号
US06946454B2

関連ノート

読み込み中…