Methyl iodide → 3-(4-Chloro-benzenesulfonyl)-3-methyl-dihydrofuran-2-one

HRID 1924859

反応式

HRID 1924859 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH:11]2[CH2:15][CH2:14][O:13][C:12]2=[O:16])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[H-].[Na+].I[CH3:20]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([C:11]2([CH3:20])[CH2:15][CH2:14][O:13][C:12]2=[O:16])(=[O:10])=[O:9])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 567327883-(4-Chlorobenzenesulfonyl)-dihydro-furan-2-one

生成物 1

HCID 582805743-(4-Chloro-benzenesulfonyl)-3-methyl-dihydrofuran-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 3-(4-chlorobenzenesulfonyl)-dihydro-furan-2-one (0.599 g; 2.29 mmol) in DMF (5 mL) at 0-5° C. was added portionwise NaH (0.23 g of a 60% dispersion in mineral oil; 5.74 mmol). The mixture stirred 30 minutes and iodomethane (0.43 mL; 6.89 mmol) was added. The reaction warmed to room temperature while stiffing overnight and was quenched with water. The solid was filtered and dried in vacuo to provide the desired product. Wt 0.488 g. 1H NMR (CDCl3) δ 7.82 (d, 2H), 7.56 (d, 2H), 4.56 (m, 1H), 4.39 (m, 1H), 3.32 (m, 1H), 2.42 (m, 1H), 1.51 (s, 3H).

後処理

  1. waitwhile stiffing overnight
  2. customwas quenched with water
  3. filtrationThe solid was filtered
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-c6143190dc594a5cb2265798165d8af5
出典データセット
uspto-grants-2012_05
特許番号
US08178568B2

関連ノート

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