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

HRID 448720

反応式

HRID 448720 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

HCID 58555336HCID 58555336、化合物収率 63%

試薬・触媒・溶媒 3

HCID 174Ethylene Glycol溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-002e91b8aab2440aa2b2282d28b739de
出典データセット
uspto-grants-2013_07
特許番号
US08481736B2

関連ノート

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