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m-Chloroperbenzoic acid → 4-[5-(3-Methyl-5-{[4-(methylsulfinyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-1,4-diazepan-2-one

HRID 1028138
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HRID 1028138 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([C:17]2[S:21][C:20]([N:22]3[CH2:28][CH2:27][CH2:26][NH:25][C:24](=[O:29])[CH2:23]3)=[N:19][CH:18]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:14]=[C:13]([S:15][CH3:16])[CH:12]=[CH:11][N:10]=2)[CH:7]=1.ClC1C=CC=C(C(OO)=[O:38])C=1>ClCCl.[O-]S([O-])(=S)=O.[Na+].[Na+]>[CH3:1][C:2]1[CH:3]=[C:4]([C:17]2[S:21][C:20]([N:22]3[CH2:28][CH2:27][CH2:26][NH:25][C:24](=[O:29])[CH2:23]3)=[N:19][CH:18]=2)[CH:5]=[C:6]([NH:8][C:9]2[N:14]=[C:13]([S:15]([CH3:16])=[O:38])[CH:12]=[CH:11][N:10]=2)[CH:7]=1
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5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 67239865HCID 67239865, 화합물

생성물 1

HCID 532512384-[5-(3-Methyl-5-{[4-(methylsulfinyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-1,4-diazepan-2-one수율 6.4%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 24477Sodium Thiosulfate용매

실험 절차

To 4-[5-(3-methyl-5-{[4-(methylsulfanyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-1,4-diazepan-2-one (50 mg, 0.117 mmol) stirring in dichloromethane (586 μL) at room temperature was added 3-chloroperbenzoic acid (27.6 mg, 0.123 mmol). Stirred for 3 hr. at room temperature, diluted with 10% Na2S2O3 (aq.), and washed with sat. NaHCO3 (aq.) and brine. The organic extracts were dried (Na2SO4), filtered, and concentrated in vacuo. Purified by reverse phase preparative HPLC (0:100 to 95:5 acetonitrile:water: 0.1% v/v trifluoroacetic acid modifier) to afford 4-[5-(3-methyl-5-{[4-(methylsulfinyl)pyrimidin-2-yl]amino}phenyl)-1,3-thiazol-2-yl]-1,4-diazepan-2-one (3.3 mg, 7.5 μmol, 6.36% yield) as a yellow solid. MS APCI: [M+H]+ m/z 443.1. 1H NMR (500 MHz, CDCl3) δ 8.67 (d, J=4.9 Hz, 1H), 7.68 (s, 1H), 7.48 (s, 1H), 7.44 (d, J=4.9 Hz, 1H), 7.34-7.29 (m, 1H), 7.19 (s, 1H), 6.96 (s, 1H), 5.93-5.85 (m, 1H), 4.28 (s, 2H), 3.46 (s, 2H), 2.93 (s, 2H), 2.37 (s, 3H), 2.16-2.01 (m, 2H), 1.25 (s, 3H). rhSYK activity=+++.

후처리

  1. washwashed with sat. NaHCO3 (aq.) and brine
  2. dry with materialThe organic extracts were dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurified by reverse phase preparative HPLC (0:100 to 95:5 acetonitrile:water: 0.1% v/v trifluoroacetic acid modifier)

출처 및 근거

ORD 기록
ord-c6a592f66590427bb1f81754e687aab0
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735417B2

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