Benzyl 6-[3-(1-adamantyl)-4-methoxycarbonylmethyloxyphenyl]-2-naphthoate → 6-[3-(1-Adamantyl)-4-methoxycarbonylmethyloxyphenyl]-2-naphthoic acid

HRID 1078494

반응식

HRID 1078494 반응식
[C:1]12([C:11]3[CH:12]=[C:13]([C:23]4[CH:24]=[C:25]5[C:30](=[CH:31][CH:32]=4)[CH:29]=[C:28]([C:33]([O:35]CC4C=CC=CC=4)=[O:34])[CH:27]=[CH:26]5)[CH:14]=[CH:15][C:16]=3[O:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.[H][H]>[Pd].O1CCOCC1.C(O)(=O)C>[C:1]12([C:11]3[CH:12]=[C:13]([C:23]4[CH:24]=[C:25]5[C:30](=[CH:31][CH:32]=4)[CH:29]=[C:28]([C:33]([OH:35])=[O:34])[CH:27]=[CH:26]5)[CH:14]=[CH:15][C:16]=3[O:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[CH2:10][CH:5]3[CH2:4][CH:3]([CH2:9][CH:7]([CH2:6]3)[CH2:8]1)[CH2:2]2

참가 물질

5

반응물 2

HCID 19429712Benzyl 6-[3-(1-adamantyl)-4-methoxycarbonylmethyloxyphenyl]-2-naphthoateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 194296986-[3-(1-Adamantyl)-4-methoxycarbonylmethyloxyphenyl]-2-naphthoic acid수율 82.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 22565020HOAc dioxane용매

실험 절차

4.24 g (7.58 mmol) of the diester obtained in Example 4 in solution in the dioxane/acetic acid mixture (99/1) are treated with 800 mg of Pd-C (10%) at a pressure of 7 bar of hydrogen at 40° C. for 6 h. The reaction medium is then filtered on celite, evaporated, washed with water and recrystallized from the acetate/tetrahydrofuran mixture. 2.94 g (82%) of a solid are isolated, which solid melts at 283°-285° C.

후처리

  1. filtrationThe reaction medium is then filtered on celite
  2. customevaporated
  3. washwashed with water
  4. customrecrystallized from the acetate/tetrahydrofuran mixture

출처 및 근거

ORD 기록
ord-6005b2658cf24b6dae5e845947ec80d1
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05547983

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