Bromosuccinimide → 3-[1-(5-Bromo-2-thienyl)cyclobutyl]-5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocine

HRID 503005

반응식

HRID 503005 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1([C:10]2[N:14]3[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:13]3=[N:12][N:11]=2)[CH2:9][CH2:8][CH2:7]1.[Br:21]C1CC(=O)NC1=O>C(O)(=O)C.C(Cl)(Cl)Cl>[Br:21][C:5]1[S:1][C:2]([C:6]2([C:10]3[N:14]4[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][C:13]4=[N:12][N:11]=3)[CH2:7][CH2:8][CH2:9]2)=[CH:3][CH:4]=1

참가 물질

5

반응물 2

HCID 38309BromosuccinimideHCID 68466191HCID 68466191, 화합물

생성물 1

HCID 684658823-[1-(5-Bromo-2-thienyl)cyclobutyl]-5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocine수율 78.5%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6212Chloroform용매

실험 절차

3-[1-(2-Thienyl)cyclobutyl]-5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocine (60 mg) was dissolved in acetic acid (3 ml) and then bromosuccinimide (38 mg) was added, followed by stirring at room temperature for 8 hours under light-shielding. The reaction solution was diluted with chloroform (30 ml) and then washed with water (10 ml), a 1M aqueous sodium hydroxide solution (10 ml), and brine (10 ml). The organic layer was dried and then concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography (methanol:chloroform=2:98) to obtain 60 mg of 3-[1-(5-bromo-2-thienyl)cyclobutyl]-5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocine (white solid).

후처리

  1. washwashed with water (10 ml)
  2. customThe organic layer was dried
  3. concentrationconcentrated under reduced pressure
  4. customthe resulting residue was purified by silica gel column chromatography (methanol:chloroform=2:98)

출처 및 근거

ORD 기록
ord-72dbb5a19d0949718cf21036bed37a53
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776897B2

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