Hydrochloric Acid → 1-(9-Methyl-5,7,8,9-tetrahydro-6H-pyrido[3',4':4,5]pyrrolo[2,3-b]pyridin-2-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one hydrochloride

HRID 882044노트

반응식

HRID 882044 반응식
[CH3:1][N:2]1[C:6]2=[N:7][C:8]([N:11]3[CH:16]=[CH:15][C:14]([C:17]4[CH:22]=[CH:21][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:19][CH:18]=4)=[CH:13][C:12]3=[O:27])=[CH:9][CH:10]=[C:5]2[C:4]2[CH2:28][NH:29][CH2:30][CH2:31][C:3]1=2.[ClH:32]>CO>[ClH:32].[CH3:1][N:2]1[C:6]2=[N:7][C:8]([N:11]3[CH:16]=[CH:15][C:14]([C:17]4[CH:18]=[CH:19][C:20]([C:23]([F:26])([F:25])[F:24])=[CH:21][CH:22]=4)=[CH:13][C:12]3=[O:27])=[CH:9][CH:10]=[C:5]2[C:4]2[CH2:28][NH:29][CH2:30][CH2:31][C:3]1=2

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 573839591-(9-Methyl-5,7,8,9-tetrahydro-6H-pyrido[3',4':4,5]pyrrolo[2,3-b]pyridin-2-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one

생성물 1

HCID 679700521-(9-Methyl-5,7,8,9-tetrahydro-6H-pyrido[3',4':4,5]pyrrolo[2,3-b]pyridin-2-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one hydrochloride수율 82%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of 1-(9-methyl-5,7,8,9-tetrahydro-6H-pyrido[3′,4′:4,5]pyrrolo[2,3-b]pyridin-2-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one (50 mg, 0.12 mmol) in MeOH (2.0 mL) was treated with 1.25 M HCl in MeOH (94 μL, 0.12 mmol), and the resulting solution was stirred at ambient temperature for 18 h. The solution was concentrated to dryness to provide the title compound (45 mg, 82%) as a bright yellow powder: mp 278-281° C. decomp.; 1H NMR (500 MHz, DMSO-d6) δ 8.06-8.00 (m, 4H), 7.88 (d, J=8.0 Hz, 2H), 7.42 (d, J=3.0 Hz, 1H), 6.90 (d, J=2.0 Hz, 1H), 6.78 (dd, J=7.0, 2.0 Hz, 1H), 4.19 (s, 2H), 3.71 (s, 3H), 3.37 (t, J=5.5 Hz, 2H), 2.99 (t, J=5.5 Hz, 2H); ESI MS m/z 425 [M+H]+; HPLC (Method A) 98.9% (AUC), tR=14.8 min.

후처리

  1. concentrationThe solution was concentrated to dryness

출처 및 근거

ORD 기록
ord-6ff6f3e189d743068895716fc1ccf05b
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993765B2

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