Piperonylamine → 1-Phenyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

HRID 647942노트

반응식

HRID 647942 반응식
Cl.[NH:2]([C:4]1[CH:5]=[CH:6][C:7]2[S:11][CH:10]=[C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:8]=2[CH:18]=1)N.O.Cl.[NH:21]1[CH2:26][CH2:25][C:24](=O)[CH2:23][CH2:22]1>C(O)(C)C>[C:12]1([C:9]2[C:8]3=[C:18]4[C:4](=[CH:5][CH:6]=[C:7]3[S:11][CH:10]=2)[NH:2][C:24]2[CH2:25][CH2:26][NH:21][CH2:22][C:23]4=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 2723901PiperonylamineHCID 204842955-Hydrazino-3-phenylbenzothiophene hydrochloride

생성물 1

HCID 204843051-Phenyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

28 g of 5-hydrazino-3-phenylbenzothiophene hydrochloride are dissolved in 300 ml of isopropanol and the solution is combined with 20 g of 4-piperidone hydrochloride monohydrate under an inert gas. After boiling the mixture for 3 hours, the solvent is evaporated off, the residue is taken up in isopropanol and the product is precipitated with the addition of isopropyl ether. The precipitate is filtered off and taken up in water; a layer of methylene chloride is introduced under the solution and the mixture is shaken with NaOH solution. The organic phase is separated off and worked up. Melting point: 228° C. (decomposition)

후처리

  1. customfor 3 hours
  2. customthe solvent is evaporated off
  3. customthe product is precipitated with the addition of isopropyl ether
  4. filtrationThe precipitate is filtered off
  5. additiona layer of methylene chloride is introduced under the solution
  6. customThe organic phase is separated off

출처 및 근거

ORD 기록
ord-241ef8d045ff4f6b9001c250146e9c54
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410536

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