Sodium hydride → 7-Fluoro-3,4-dihydro-1-benzoxepin-5(2H)-one

HRID 708262노트

반응식

HRID 708262 반응식
[H-].[Na+].Br[CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[C:14](=[O:16])[CH3:15]>C1COCC1>[F:13][C:10]1[CH:11]=[CH:12][C:7]2[O:6][CH2:5][CH2:4][CH2:15][C:14](=[O:16])[C:8]=2[CH:9]=1

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 58203950HCID 58203950, 화합물

생성물 1

HCID 122435647-Fluoro-3,4-dihydro-1-benzoxepin-5(2H)-one수율 56.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Weighed out Sodium Hydride (561 mg, 23.4 mmol) into a nitrogen purged round bottom flask and added 10 mL THF. Placed the solution under nitrogen and added 1-(2-(2-bromoethoxy)-5-fluorophenyl)ethanone (4.07 g, 15.6 mmol) in 15 mL THF. Let stir at room temperature overnight. Concentrated in vacuo and flashed 0 to 50% ethyl acetate/hexanes. NMR confirmed product as 7-fluoro-3,4-dihydrobenzo[b]oxepin-5(2H)-one (1.58 g, 56.2% yield).

후처리

  1. concentrationConcentrated in vacuo

출처 및 근거

ORD 기록
ord-7a616765022840f990559389c30c083f
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175009B2

반응 노트

불러오는 중…