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Triethylamine → Methyl 2-(6,7-dimethoxy-1,2-dihydronaphthalene-3-carboxamido)benzoate

HRID 2175708
ノート
印刷プレビュー

反応式

HRID 2175708 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].CCN(CC)CC.[CH3:19][O:20][C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][C:30]=1[O:31][CH3:32])[CH:27]=[C:26]([C:33](Cl)=[O:34])[CH2:25][CH2:24]2>C(Cl)Cl>[CH3:32][O:31][C:30]1[CH:29]=[C:28]2[C:23](=[CH:22][C:21]=1[O:20][CH3:19])[CH2:24][CH2:25][C:26]([C:33]([NH:1][C:2]1[CH:11]=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])=[O:34])=[CH:27]2
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 8471TriethylamineHCID 8635Methyl AnthranilateHCID 103548826,7-dimethoxy-3,4-dihydronaphthalene-2-carbonyl Chloride

生成物 1

HCID 67087821Methyl 2-(6,7-dimethoxy-1,2-dihydronaphthalene-3-carboxamido)benzoate収率 45%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 6,7-dimethoxy-3,4-dihydronaphthalene-2-carboxylic acid (476 mg, 2 mmol) and SOCl2 (1.5 mL, 20 mmol) in toluene (20 mL) was heated at 50° C. for 1 hour. The solvent was then removed under reduced pressure to give 6,7-dimethoxy-3,4-dihydronaphthalene-2-carbonyl chloride which was used directly in the next step without further purification. To a stirred solution of methyl 2-aminobenzoate (332 mg, 2.2 mmol) and Et3N (0.8 mL, 6 mmol) in anhydrous DCM (20 mL) was added 6,7-dimethoxy-3,4-dihydronaphthalene-2-carbonyl chloride in anhydrous DCM (2 mL) dropwise at 0° C. The resulting mixture was stirred at room temperature overnight. The reaction was quenched with water and extracted with DCM. The combined organic phase was dried over sodium sulfate, the solvent was removed under reduced pressure and the residue was purified by flash column, eluting with petroleum ether/ethyl acetate (10:1) to give methyl 2-(6,7-dimethoxy-1,2-dihydronaphthalene-3-carboxamido)benzoate (330 mg, 45%). LC-MS (ES-API); rt 9.27 min; m/z calculated for C21H21NO5 [M+Na]+ 390.1, found 390.1.

後処理

  1. customwas used directly in the next step without further purification
  2. customThe reaction was quenched with water
  3. extractionextracted with DCM
  4. dry with materialThe combined organic phase was dried over sodium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customthe residue was purified by flash column
  7. washeluting with petroleum ether/ethyl acetate (10:1)

出典と根拠

ORDレコード
ord-8cb4196919a3427590018dfde6738cb6
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09062076B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート