Methyl iodide → 7-methoxy-3,4-dihydro-2H-1-benzopyran-4-one

HRID 510712노트

반응식

HRID 510712 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[CH2:7][CH2:8][O:9]2)=[CH:4][CH:3]=1.[C:13]([O-])([O-])=O.[K+].[K+].CI>O1CCCC1>[CH3:13][O:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[CH2:7][CH2:8][O:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 108558177-hydroxy-2,3-dihydro-4H-chromen-4-one

생성물 1

HCID 43875107-methoxy-3,4-dihydro-2H-1-benzopyran-4-one수율 72.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

7-Hydroxy-2,3-dihydrochromen-4-one (4.47 g, 27.2 mmol) was diluted with tetrahydrofuran (40 mL) followed by the addition of K2CO3 (5.64 g, 40.8 mmol) and MeI (2.55 mL, 40.8 mmol). The reaction was heated at 70° C. for 5 hours. The reaction was allowed to cool and loaded onto a Biotage 40M cartridge running a gradient 5% ethyl acetate/hexanes to 75% to yield the title compound (3.5 g, 72.1% yield).

후처리

  1. temperatureto cool

출처 및 근거

ORD 기록
ord-a05cc1df11e44cfaa04295f288410ea7
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096567B2

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