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1,1'-(Diazomethylene)bis(benzene) → HCID 58928752、化合物

HRID 853694
ノート
印刷プレビュー

反応式

HRID 853694 の反応式
CCCC[N+](CCCC)(CCCC)CCCC.[F-].[CH3:19][O:20][C:21]([C:23]1[C:24]([O:48][CH3:49])=[C:25]2[C:30](=[C:31]([O:37][Si](C(C)C)(C(C)C)C(C)C)[C:32]=1[C:33]([O:35][CH3:36])=[O:34])[N:29]=[CH:28][CH:27]=[CH:26]2)=[O:22].[C:50]1([C:56]([C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=2)=[N+]=[N-])[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1>C1COCC1>[CH3:19][O:20][C:21]([C:23]1[C:24]([O:48][CH3:49])=[C:25]2[C:30](=[C:31]([O:37][CH:56]([C:50]3[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=3)[C:59]3[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=3)[C:32]=1[C:33]([O:35][CH3:36])=[O:34])[N:29]=[CH:28][CH:27]=[CH:26]2)=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 612301,1'-(Diazomethylene)bis(benzene)HCID 2724141Tetrabutylammonium FluorideHCID 589290076,7-Dimethyl 5-methoxy-8-[[tris(1-methylethyl)silyl]oxy]-6,7-quinolinedicarboxylate

生成物 1

HCID 58928752HCID 58928752、化合物収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A 1M solution of TBAF in THF (4 ml) was added to 5-methoxy-8-triisopropylsilanyloxy-quinoline-6,7-dicarboxylic acid dimethyl ester (0.85 g, 1.9 mmol) in 20 ml dry THF. The reaction was stirred at rt for 1 h, at which time the reaction mixture was concentrated and the residue dissolved in 100 mL diethyl ether and washed with 25 mL 1N HCl, followed by 25 mL of saturated aq. NaCl. The organic layer was concentrated and the residue was dissolved in 40 mL dichloroethane. Diphenyldiazomethane (0.7 g, 3.8 mmol) was added and the reaction temperature was raised to 70° C. for 24 h. The reaction mixture was concentrated and the residue chromatographed on silica gel (1/1 hexanes/EtOAc) to give 8-benzhydryloxy-5-methoxy-quinoline-6,7-dicarboxylic acid dimethyl ester (0.8 g, 61% yield overall). 1H NMR (CDCl3) δ 8.85 (d, 1H), 8.45 (d, 1H), 7.45 (dd, 1H), 3.98 (s, 3H), 3.85 (s, 3H), 3.74 (s, 3H); MS: 480 (M+Na).

後処理

  1. concentrationwas concentrated
  2. dissolutionthe residue dissolved in 100 mL diethyl ether
  3. washwashed with 25 mL 1N HCl
  4. concentrationThe organic layer was concentrated
  5. dissolutionthe residue was dissolved in 40 mL dichloroethane
  6. temperaturethe reaction temperature was raised to 70° C. for 24 h
  7. concentrationThe reaction mixture was concentrated
  8. customthe residue chromatographed on silica gel (1/1 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-9d1649460adc40c99dc5f65bf34be258
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07253180B2

反応ノート

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