11-Methylene-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic acid → 11-Methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid

HRID 894220노트

반응식

HRID 894220 반응식
[CH2:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2>[Pd].C(O)C>[CH3:1][CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2

참가 물질

4

반응물 1

HCID 1292913311-Methylene-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic acid

생성물 1

HCID 1292913411-Methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid수율 70.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Dissolve 514 mg of 11-methylene-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic acid in 150 ml. of ethanol. Add 100 mg of 5% palladium on carbon catalyst. Hydrogenate at 20 psi for 30 minutes. Filter and strip the filtrate to dryness. Recrystallize the residue from isopropanol to obtain the title product (yield 365 mg, m.p. 224°-226° C.).

후처리

  1. filtrationFilter
  2. customRecrystallize the residue from isopropanol

출처 및 근거

ORD 기록
ord-5c4ef8f90bd149b48d2a71d8c3ea4744
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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