Methanesulfonyl chloride → N-[4-(4-Chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenyl]-methanesulfonamide

HRID 629009ノート

反応式

HRID 629009 の反応式
[Cl:1][C:2]1[C:7]([S:8][CH3:9])=[C:6]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[N:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][CH:17]=2)[N:3]=1.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>C(Cl)Cl>[Cl:1][C:2]1[C:7]([S:8][CH3:9])=[C:6]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[N:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([NH:22][S:24]([CH3:23])(=[O:26])=[O:25])=[CH:18][CH:17]=2)[N:3]=1

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 86673495HCID 86673495、化合物

生成物 1

HCID 86673496N-[4-(4-Chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenyl]-methanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 4-(4-chloro-5-methylsulfanyl-6-morpholin-4-yl-pyrimidin-2-yl)-phenylamine (30 mg, 0.091 mmol.), methanesulfonyl chloride (15.5 mg, 0.136 mmol, 1.5 eq.) and CH2Cl2 was added to the reaction vessel and flushed with argon. The reaction mixture was stirred at r.t. for 2 hrs. The reaction mixture was partitioned between CH2Cl2 and NaHCO3 (aq), the organic layer was washed with brine, dried over MgSO4, filtered and evaporated in vacuo. A white solid of 30.3 mg (82.1%) was obtained as the product.

後処理

  1. additionwas added to the reaction vessel
  2. customflushed with argon
  3. customThe reaction mixture was partitioned between CH2Cl2 and NaHCO3 (aq)
  4. washthe organic layer was washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customA white solid of 30.3 mg (82.1%) was obtained as the product

出典と根拠

ORDレコード
ord-69b170ead6e84c82943c147b07956a80
出典データセット
uspto-grants-2016_04
特許番号
US09315491B2

反応ノート

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