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Water → HCID 66612048、化合物

HRID 1621873
ノート
印刷プレビュー

反応式

HRID 1621873 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 66611542HCID 66611542、化合物HCID 131730192HCID 131730192、化合物

生成物 1

HCID 66612048HCID 66612048、化合物収率 71.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b8513de061bc4b5685ca7b199cd7b1e6
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772480B2

反応ノート

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