Methanol → HCID 68776598, 화합물

HRID 2217603

반응식

HRID 2217603 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]=[C:12]([C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=2)[C:13]([OH:15])=[O:14])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.S(=O)(=O)(O)O.[CH3:28]O>>[CH3:28][O:14][C:13](=[O:15])[C:12]([C:16]1[CH:17]=[CH:18][C:19]([OH:22])=[CH:20][CH:21]=1)=[CH:11][C:5]1[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 3567513-(3,5-Dimethoxyphenyl)-2-(4-hydroxyphenyl)-acrylic acid

생성물 1

HCID 68776598HCID 68776598, 화합물

실험 절차

Methanol (3.0 L) was added to a thoroughly dried 7 (427.5 g, 1.42 mol) under argon. To this stirred suspension concentrated sulfuric acid (100 mL) was added and heated at reflux for 20 h under nitrogen. Methanol was evaporated under reduced pressure at 30° C. The residue was taken up in ethyl acetate (3.0 L) and washed with water (2×1.0 L), saturated aqueous Na HCO3 (2×1.0 L), brine (2×1.0 L). The organic layer was dried on anhydrous magnesium sulfate, filtered and the solvent was evaporated. The residue obtained was dried thoroughly under high vacuum as white solid, (433.6 g 97%): mp 106-108° C.; 1HNMR(360 MHz, CDCl3): δ 7.72 (s, 1H), 7.06 (d, J=7.9 Hz, 2H), 6.77 (d, J=7.9 Hz, 2H), 6.33 (t, J=2.2 Hz, 1H), 6.26 (d, J=2.2 Hz, 2H), 5.74 (s, 1H), 3.81 (s, 3H), 3.60 (s, 6H); MS (EI) m/z 315[M]+; Anal. (C18H18O5) C, H.

후처리

  1. temperatureheated
  2. temperatureat reflux for 20 h under nitrogen
  3. customMethanol was evaporated under reduced pressure at 30° C
  4. washwashed with water (2×1.0 L), saturated aqueous Na HCO3 (2×1.0 L), brine (2×1.0 L)
  5. dry with materialThe organic layer was dried on anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue obtained
  9. customwas dried thoroughly under high vacuum as white solid, (433.6 g 97%)

출처 및 근거

ORD 기록
ord-9d33c2d6c2db420b947d6d45b828a47e
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07407978B2

연결된 노트

불러오는 중…