HCID 22452664, 화합물 → HCID 22452628, 화합물

HRID 2185905노트

반응식

HRID 2185905 반응식
[CH:1]([O:4][C:5]1[CH:6]=[C:7]([C:15]([OH:17])=[O:16])[C:8]2[C:13]([CH:14]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)([CH3:3])[CH3:2]>CC(O)=O.[Pd]>[CH:1]([O:4][C:5]1[CH:6]=[C:7]([C:15]([OH:17])=[O:16])[C:8]2[CH2:9][CH2:10][CH2:11][CH2:12][C:13]=2[CH:14]=1)([CH3:3])[CH3:2]

참가 물질

4

반응물 1

HCID 22452664HCID 22452664, 화합물

생성물 1

HCID 22452628HCID 22452628, 화합물수율 100.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

A mixture of 3-(isopropoxy)-1-naphthalenecarboxylic acid (0.38 g, 1.65 mmol) and 10% Pd/C (0.10 g) in HOAc (20 mL) was hydrogenated on Parr apparatus at 60° C. and 50 psi for 13 h. After filtration through diatomaceous earth the solvent was removed in vacuo, water was added and the precipitate was extracted into EtOAc. The combined organic layers were dried (MgSO4), filtered and concentrated to yield the title acid as a light yellow oil (0.39 g, 100%). 1H NMR (CDCl3) δ 7.39 (d, 1H), 6.83 (d, 1H), 4.55 (m, 1H), 3.02 (s, 2H), 2.80 (s, 2H), 1.77 (m, 4H), 1.34 (s, 3H), 1.32 (s, 3H); MS m/z 233 (M−H).

후처리

  1. customwas hydrogenated on Parr apparatus at 60° C.
  2. filtrationAfter filtration through diatomaceous earth the solvent
  3. customwas removed in vacuo, water
  4. additionwas added
  5. extractionthe precipitate was extracted into EtOAc
  6. dry with materialThe combined organic layers were dried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-393d04bbbaa14af7be5f1b6adc18c252
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06403601B1

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