1H,3H-Naphtho(1,8-cd)pyran-1,3-dione, 6-bromo- → HCID 58555336, 화합물

HRID 448720

반응식

HRID 448720 반응식
[Br:1][C:2]1[C:11]2[C:6]3=[C:7]([C:12]([O:14][C:15](=[O:16])[C:5]3=[CH:4][CH:3]=1)=O)[CH:8]=[CH:9][CH:10]=2.[CH2:17]([CH:24]([NH2:32])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]>C(O)CO.CO.O>[CH2:17]([CH:24]([N:32]1[C:12](=[O:14])[C:7]2=[C:6]3[C:11](=[CH:10][CH:9]=[CH:8]2)[C:2]([Br:1])=[CH:3][CH:4]=[C:5]3[C:15]1=[O:16])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]

참가 물질

6

반응물 2

HCID 664931H,3H-Naphtho(1,8-cd)pyran-1,3-dione, 6-bromo-HCID 2329078-Pentadecanamine

생성물 1

HCID 58555336HCID 58555336, 화합물수율 63%

시약·촉매·용매 3

HCID 174Ethylene Glycol용매HCID 887Methanol용매HCID 962Water용매

실험 절차

5 g (18 mmol) of 4-bromonaphthalene-1,8-dicarboxylic anhydride were heated to 160° C. with 6.1 g (27 mmol) of 1-heptyloctylamine in 50 ml of ethylene glycol for 4 hours. The resulting solution was allowed to cool to room temperature. Thereafter, the solution was diluted with 50 ml of methanol and 50 ml of distilled water. The aqueous solution was extracted with diethyl ether, the solution was dried over MgSO4 and the solvent was evaporated. The resulting yellow oil was purified by column chromatography with dichloromethane as the eluent, which afforded 5.5 g (63%) of the title compound as a colorless oil.

후처리

  1. extractionThe aqueous solution was extracted with diethyl ether
  2. dry with materialthe solution was dried over MgSO4
  3. customthe solvent was evaporated
  4. customThe resulting yellow oil was purified by column chromatography with dichloromethane as the eluent, which

출처 및 근거

ORD 기록
ord-002e91b8aab2440aa2b2282d28b739de
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481736B2

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