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Hydrochloric Acid → Trifluoroacetic acid

HRID 1043467
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HRID 1043467 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH3:8][C:9]1[N:13](C2CCCCO2)[N:12]=[C:11]([C:20]([F:23])([F:22])[F:21])[C:10]=1[C:24]1[NH:25][C:26]2[C:32]3[CH:33]=[CH:34][N:35]=[CH:36][C:31]=3[NH:30][C:29]3[N:37]=[CH:38][CH:39]=[CH:40][C:28]=3[C:27]=2[N:41]=1.Cl>CO>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH3:8][C:9]1[NH:13][N:12]=[C:11]([C:20]([F:23])([F:22])[F:21])[C:10]=1[C:24]1[NH:25][C:26]2[C:32]3[CH:33]=[CH:34][N:35]=[CH:36][C:31]=3[NH:30][C:29]3[N:37]=[CH:38][CH:39]=[CH:40][C:28]=3[C:27]=2[N:41]=1.[C:3]([OH:5])([C:2]([F:7])([F:6])[F:1])=[O:4]
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 866132712-[5-methyl-1-(tetrahydro-2H-pyran-2-yl)-3-(trifluoromethyl)-1H-pyrazol-4-yl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepine trifluoroacetate

생성물 2

HCID 6422Trifluoroacetic acid수율 1,172.2%HCID 866132702-[5-methyl-3-(trifluoromethyl)-1H-pyrazol-4-yl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepine bis(trifluoroacetate)

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a solution of 2-[5-methyl-1-(tetrahydro-2H-pyran-2-yl)-3-(trifluoromethyl)-1H-pyrazol-4-yl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b: 4′,3′-f]azepine trifluoroacetate (715 mg, 1.23 mmol) in methanol (16 mL) was added 1.25 mL concentrated HCl and the reaction was stirred at 50° C. for 3 h. The reaction was reduced in vacuo and then purified by preparative LCMS to obtain the desired product as a bis-TFA salt (548 mg, 73%). 1H NMR (400 MHz, DMSO-d6): δ 13.8 (bs, 1H), 8.60 (bs, 1H), 8.10 (d, 1H), 8.01 (s, 1H), 7.94 (dd, 1H), 7.61 (m, 2H), 6.88 (dd, 1H), 2.35 (s, 3H). 19F NMR (400 MHz, DMSO-d6): δ −59.476 (3F), −74.791 (6F). MS (EI) m/z=384. (M+H).

후처리

  1. custompurified by preparative LCMS

출처 및 근거

ORD 기록
ord-0563cfeedc2444f5bf8940cffe80a621
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08563541B2

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