Methanesulfonic Acid → 1-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonate

HRID 1742957

반응식

HRID 1742957 반응식
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:15]4[CH2:19][CH2:18][CH:17]([N:20]5[CH:24]=[N:23][CH:22]=[N:21]5)[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:26])[C:6]([C:27]([OH:29])=[O:28])=[CH:5]2)[CH2:3][CH2:2]1.[CH3:30][S:31]([OH:34])(=[O:33])=[O:32]>C(Cl)(Cl)Cl>[CH3:30][S:31]([OH:34])(=[O:33])=[O:32].[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:25])=[C:11]([N:15]4[CH2:19][CH2:18][CH:17]([N:20]5[CH:24]=[N:23][CH:22]=[N:21]5)[CH2:16]4)[C:12]=3[F:14])[C:7](=[O:26])[C:6]([C:27]([OH:29])=[O:28])=[CH:5]2)[CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 190059571-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

생성물 1

HCID 867480961-Cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol-1-yl) pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid methanesulfonate

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

1-cyclopropyl-6,8-difluoro-7-[3-(1,2,4-triazol -1-yl)pyrrolidin-1-yl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (20 mg, 0.05 mmol) was dissolved in 2 ml of chloroform and to this was added 4 ml of methanesulfonic acid in chloroform. The suspension formed was stirred at room temperature for five hr. The solid was collected to yield 12 mg of white solid after drying very well in the oven, m.p. 208.5°-210° C. 1H NMR (CD3OD) δ: 9.54 (s, 1H), 8.78 (s, 1H), 8.64 (s, 1H), 7.81 (dd, 13.8, 2.3Hz, 1H), 5.47-5.3 (m, 1H), 4.5-3.8 (m, 5H), 2.88-2.5 (m, 2H), 2.7 (s, 3H), 1.4-1.1 (m, 4H). Anal. calcd. for C20H21F2N5O6S . H2O: C, 46.60; H, 4.50; N, 13.59.Found: C, 46.75; H, 4.38; N, 13.51.

후처리

  1. customThe suspension formed
  2. customThe solid was collected

출처 및 근거

ORD 기록
ord-2b08be761698415f88627290a75c638f
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05342846

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