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HCID 68144627, 화합물 → 13-Ethyl-3-methoxy-6-methylgona-1,3,5(10)-trien-17-one

HRID 1415048
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HRID 1415048 반응식
[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH:13]=[CH:14][C:15]([O:21][CH3:22])=[CH:16][C:17]=4[CH:18]([CH3:20])[CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C:4]12OCC[O:23]1)[CH3:2]>CO.Cl>[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH:13]=[CH:14][C:15]([O:21][CH3:22])=[CH:16][C:17]=4[CH:18]([CH3:20])[CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C:4]2=[O:23])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 68144627HCID 68144627, 화합물

생성물 1

HCID 6814340513-Ethyl-3-methoxy-6-methylgona-1,3,5(10)-trien-17-one수율 92.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

Suspend dl-13-ethyl-3-methoxy-6-methyl-17,17-ethylenedioxygona-1,3,5(10)-triene (9.0 g) in methanol (200 ml) and concentrated hydrochloric acid (5 ml). Heat the mixture on a steam bath for 15 minutes. Remove the solvent under vacuum and partition the residue between ether and aqueous sodium bicarbonate. Remove the organic solvents and dry to obtain a gum. Recrystallize from methanol to obtain dl-13-ethyl-3-methoxy-6-methylgona-1,3,5(10)-trien-17-one (7.29 g), m.p. 115°-123°. Recrystallize from methanol to obtain an analytical sample with m.p. 123°-127°; ultraviolet absorption peak at 280 mμ (ε2,190), infrared maximum (potassium bromide) at 5.75 μ.

후처리

  1. temperatureHeat the mixture on a steam bath for 15 minutes
  2. customRemove the solvent under vacuum
  3. custompartition the residue between ether and aqueous sodium bicarbonate
  4. customRemove the organic solvents
  5. customdry
  6. customto obtain a gum
  7. customRecrystallize from methanol

출처 및 근거

ORD 기록
ord-9211039b1ee841819b5e2eaed2675cfd
출처 데이터셋
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04002746

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