m-Chloroperbenzoic acid → 3-(1,3-Benzoxazol-2-yl)-5-[1-(1-methyl-1-oxido-piperidin-1-ium-4-yl)pyrazol-4-yl]pyridin-2-amine

HRID 908375노트

반응식

HRID 908375 반응식
ClC1C=C(C(OO)=[O:9])C=CC=1.[O:12]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[C:13]1[C:21]1[C:22]([NH2:39])=[N:23][CH:24]=[C:25]([C:27]2[CH:28]=[N:29][N:30]([CH:32]3[CH2:37][CH2:36][N:35]([CH3:38])[CH2:34][CH2:33]3)[CH:31]=2)[CH:26]=1>C(Cl)Cl>[O:12]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[C:13]1[C:21]1[C:22]([NH2:39])=[N:23][CH:24]=[C:25]([C:27]2[CH:28]=[N:29][N:30]([CH:32]3[CH2:33][CH2:34][N+:35]([CH3:38])([O-:9])[CH2:36][CH2:37]3)[CH:31]=2)[CH:26]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 425993593-(1,3-Benzoxazol-2-yl)-5-[1-(1-methyl-4-piperidyl)pyrazol-4-yl]pyridin-2-amine

생성물 1

HCID 866301463-(1,3-Benzoxazol-2-yl)-5-[1-(1-methyl-1-oxido-piperidin-1-ium-4-yl)pyrazol-4-yl]pyridin-2-amine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Chlorobenzenecarboperoxoic acid (0.046 g) was added to 3-(1,3-benzoxazol-2-yl)-5-[1-(1-methyl-4-piperidyl)pyrazol-4-yl]pyridin-2-amine (0.100 g) in DCM (10 ml). The resulting solution was stirred for 5 minutes. The resultant precipitate was collected by filtration, washed with DCM (2 ml) and dried under vacuum. The residue was purified by SCX ion exchange chromatography (elution with 7M methanolic ammonia) and there was thus obtained 3-(1,3-benzoxazol-2-yl)-5-[1-(1-methyl-1-oxido-piperidin-1-ium-4-yl)pyrazol-4-yl]pyridin-2-amine (0.026 g); Mass Spectrum: M+H+ 391.29; RT 1.18 min; NMR Spectrum: (DMSOd6) 8.49 (d, 1H), 8.41 (d, 1H), 8.32 (s, 1H), 7.88 (s, 1H), 7.78 (dd, 1H), 7.73 (dd, 1H), 7.57 (br s, 2H), 7.38 (m, 2H), 4.26 (tt, 1H), 3.46 (m, 2H), 3.11 (s, 3H), 3.06 (m, 2H), 2.68 (m, 2H), 1.90 (br m, 2H).

후처리

  1. filtrationThe resultant precipitate was collected by filtration
  2. washwashed with DCM (2 ml)
  3. customdried under vacuum
  4. customThe residue was purified by SCX ion exchange chromatography (elution with 7M methanolic ammonia) and there
  5. customRT 1.18 min

출처 및 근거

ORD 기록
ord-3c94da2a089d476ca493392fe87662ff
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017611B2

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