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Water → HCID 66612048, 화합물

HRID 1812280
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HRID 1812280 반응식
[CH2:1]([S:3]([C:5]1[CH:6]=[C:7]([C:21]2[N:26]=[C:25]([CH3:27])[N:24]=[C:23]([N:28]([CH2:38][C:39]3[CH:44]=[CH:43][C:42]([O:45][CH3:46])=[CH:41][CH:40]=3)[CH2:29][C:30]3[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=3)[N:22]=2)[C:8]([NH:11][C:12]2[CH:13]=[N:14][C:15]([O:19][CH3:20])=[C:16]([F:18])[CH:17]=2)=[N:9][CH:10]=1)=[O:4])[CH3:2].O.S(O)([O-])(=O)=[O:49].S(O)(OO)(=O)=O.[K+]>CO.O1CCOCC1>[CH2:1]([S:3]([C:5]1[CH:6]=[C:7]([C:21]2[N:26]=[C:25]([CH3:27])[N:24]=[C:23]([N:28]([CH2:29][C:30]3[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][CH:31]=3)[CH2:38][C:39]3[CH:40]=[CH:41][C:42]([O:45][CH3:46])=[CH:43][CH:44]=3)[N:22]=2)[C:8]([NH:11][C:12]2[CH:13]=[N:14][C:15]([O:19][CH3:20])=[C:16]([F:18])[CH:17]=2)=[N:9][CH:10]=1)(=[O:49])=[O:4])[CH3:2]
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참가 물질

6

반응물 3

HCID 962WaterHCID 66611542HCID 66611542, 화합물HCID 131730192HCID 131730192, 화합물

생성물 1

HCID 66612048HCID 66612048, 화합물수율 71.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a slurry of 4-(5-(ethylsulfinyl)-2-(5-fluoro-6-methoxypyridin-3-ylamino)pyridin-3-yl)-N,N-bis(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine (0.090 g, 0.140 mmol) in 2 mL MeOH, 2 mL dioxane, and 1 mL water was added potassium peroxymonosulfate sulfate (0.172 g, 0.280 mmol). The bright yellow slurry was stirred rapidly overnight. The reaction was partitioned between satd NaHCO3 and DCM. The aqueous layer was extracted with DCM 3 times, and the combined organics were dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The material was treated with DCM and purified by silica gel chromatography (25 g column) using 20 to 100% EtOAc/hexane. The product-containing fractions were concentrated to afford 4-(5-(ethylsulfonyl)-2-(5-fluoro-6-methoxypyridin-3-ylamino)pyridin-3-yl)-N,N-bis(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine (0.066 g, 0.100 mmol, 71.6% yield) as a yellow solid. m/z (ESI, +ve ion) 660 (M+H)+. 1H NMR (400 MHz, CDCl3) δ 11.91 (s, 1H), 8.80 (d, J=2.7 Hz, 1H), 8.43 (d, J=2.7 Hz, 1H), 8.15-8.33 (m, 2H), 7.14-7.25 (m, 4H), 6.80-6.93 (m, 4H), 4.87 (s, 2H), 4.83 (s, 2H), 4.02 (s, 3H), 3.82 (s, 3H), 3.79 (s, 3H), 3.07-3.22 (m, 1H), 2.82-2.94 (m, 1H), 2.62 (s, 3H), 1.28 (t, J=7.4 Hz, 3H).

후처리

  1. customThe reaction was partitioned between satd NaHCO3 and DCM
  2. extractionThe aqueous layer was extracted with DCM 3 times
  3. dry with materialthe combined organics were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. additionThe material was treated with DCM
  7. custompurified by silica gel chromatography (25 g column)
  8. concentrationThe product-containing fractions were concentrated

출처 및 근거

ORD 기록
ord-1c815aa1d59a4a38ad2ee5de32ca8e26
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08362241B2

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