Hydrochloric Acid → 1'-Ethyl-5-(4'-hydrazinocarbonyl-2'-methylbiphenyl-4-carbonyl)-2,3,6,7-tetrahydrospiro[furo[2,3-f]indole-3,4'-piperidine]

HRID 1741125노트

반응식

HRID 1741125 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][C:6]2([C:19]3[C:11](=[CH:12][C:13]4[CH2:14][CH2:15][N:16]([C:20]([C:22]5[CH:27]=[CH:26][C:25]([C:28]6[CH:33]=[CH:32][C:31]([C:34]7[O:35]C(C)=[N:37][N:38]=7)=[CH:30][C:29]=6[CH3:40])=[CH:24][CH:23]=5)=[O:21])[C:17]=4[CH:18]=3)[O:10][CH2:9]2)[CH2:5][CH2:4]1)[CH3:2].Cl.CCOCC>CO>[CH2:1]([N:3]1[CH2:8][CH2:7][C:6]2([C:19]3[C:11](=[CH:12][C:13]4[CH2:14][CH2:15][N:16]([C:20]([C:22]5[CH:23]=[CH:24][C:25]([C:28]6[CH:33]=[CH:32][C:31]([C:34]([NH:38][NH2:37])=[O:35])=[CH:30][C:29]=6[CH3:40])=[CH:26][CH:27]=5)=[O:21])[C:17]=4[CH:18]=3)[O:10][CH2:9]2)[CH2:5][CH2:4]1)[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 5311426SB-236057

생성물 1

HCID 218337121'-Ethyl-5-(4'-hydrazinocarbonyl-2'-methylbiphenyl-4-carbonyl)-2,3,6,7-tetrahydrospiro[furo[2,3-f]indole-3,4'-piperidine]수율 39.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A stirred solution of 1'-ethyl-5-[2'-methyl-4'-(5-methyl-1,3,4-oxadiazol-2-yl)biphenyl-4-carbonyl]-2,3,6,7-tetrahydrospiro[furo[2,3-f]indole-3,4'-piperidine] (E26, 2.5 g, 4.7 mmole) in methanol (600 ml) was treated with 1M hydrogen chloride in ether (30 ml, 30 mmole) and kept at room temp. for 20 hours, then concentrated in vacuo. The residue was treated with 10% Na2CO3 solution (200 ml) and chloroform (500 ml), stirred well for 20 minutes, then the chloroform layer separated, dried and concentrated in vacuo. The residue was crystallised from ethyl acetate to afford the title compound as a beige solid (0.94 g, 39%) m.p. 222-225° C.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue was treated with 10% Na2CO3 solution (200 ml) and chloroform (500 ml)
  3. customthe chloroform layer separated
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customThe residue was crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-57fa90050dad4424a1f7118d76c56160
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972951

반응 노트

불러오는 중…