Hydrochloric Acid → Ethyl (1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate hydrochloride

HRID 2236093노트

반응식

HRID 2236093 반응식
C(OC([N:8]1[CH2:26][CH2:25][C:11]2[N:12]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[C:10]=2[CH2:9]1)=O)(C)(C)C.[ClH:27]>C(OCC)(=O)C>[ClH:27].[CH2:9]1[C:10]2[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:12]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:11]=2[CH2:25][CH2:26][NH:8]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 71063767Ethyl (2-tert-butoxycarbonyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate

생성물 1

HCID 71552668Ethyl (1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate hydrochloride수율 79%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of ethyl (2-tert.-butoxycarbonyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-acetate (8.45 g, 23.6 mmol) in ethyl acetate (80 ml) is treated with a solution of 3M HCl in ethyl acetate (39.3 ml). After stirring at room temperature for 3 h, the solvent is removed in vacuo and the residue azeotroped twice with toluene. The crude product is suspended in diethyl ether, filtered off, washed with diethyl ether and dried. Finally, pure title compound is obtained as beige solid (5.49 g) in 79% yield. tR (LC-2) 1.41 min; ESL-MS (positive ion): m/z 259.33 [M+H]+ (calcd 258.32 for C15H18N2O2).

후처리

  1. customthe solvent is removed in vacuo
  2. customthe residue azeotroped twice with toluene
  3. filtrationfiltered off
  4. washwashed with diethyl ether
  5. customdried

출처 및 근거

ORD 기록
ord-f773c64b2dfe498e933999e41fe0dbf4
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714132B2

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