Acetic Anhydride → 1-(2,6-dihydroxyphenyl)-2-methyl-1-propanone O-acetyloxime

반응식

[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[N:13][OH:14])[CH:10]([CH3:12])[CH3:11].[C:15](OC(=O)C)(=[O:17])[CH3:16]>>[C:15]([O:14][N:13]=[C:9]([C:3]1[C:4]([OH:8])=[CH:5][CH:6]=[CH:7][C:2]=1[OH:1])[CH:10]([CH3:12])[CH3:11])(=[O:17])[CH3:16]

참가 물질

반응물 2

HCID 7918Acetic Anhydride

HCID 1363786541-(2,6-Dihydroxyphenyl)-2-methyl-1-propanone oxime2회

생성물 1

HCID 1363786551-(2,6-dihydroxyphenyl)-2-methyl-1-propanone O-acetyloxime수율 32.7%

실험 절차

1-(2,6-dihydroxyphenyl)-2-methyl-1-propanone oxime (Intermediate 38, 320 mg) was stirred in acetic anhydride (0.928 ml, 9.84 mmol) at room temperature for 1 hour. After removal of the volatiles, the crude was washed with water, filtered and dried. The residue obtained was charged on a silica gel column (Biotage SP1 system) and eluted with Cyhexane/ethyl acetate (from 100/0 to 0/100) to afford the title compound (127 mg).

후처리

customAfter removal of the volatiles
washthe crude was washed with water
filtrationfiltered
customdried
customThe residue obtained
additionwas charged on a silica gel column (Biotage SP1 system)
washeluted with Cyhexane/ethyl acetate (from 100/0 to 0/100)

출처 및 근거

ORD 기록: ord-951341dc2bf7489ab8d50e65c3dc7e09
출처 데이터셋: uspto-grants-2016_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09346790B2

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