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

HRID 1924859

반응식

HRID 1924859 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-c6143190dc594a5cb2265798165d8af5
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178568B2

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