4-Methoxybenzylamine → HCID 57456934、化合物

HRID 2077012ノート

反応式

HRID 2077012 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=[O:12])[C:3]=1[C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14].COC1C=CC(C[NH2:30])=CC=1>CN(C=O)C.C(O)(C(F)(F)F)=O>[NH2:30][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][C:4](=[O:12])[C:3]=1[C:13]([O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:14]

参加物

5

反応物 2

HCID 754524-MethoxybenzylamineHCID 57456935Benzyl 4-chloro-2-oxo-1,2-dihydroquinoline-3-carboxylate

生成物 1

HCID 57456934HCID 57456934、化合物収率 116.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
115 °C

実験手順

Benzyl 4-chloro-2-oxo-1,2-dihydroquinoline-3-carboxylate (Example 66b) (0.55 g, 1.75 mmol) was dissolved in DMF (8 mL) and 4-methoxybenzylamine (0.56 mL, 4.31 mmol) was added. The reaction was heated at 115° C. for 30 minutes, then cooled to room temperature and poured into ice water. The resultant precipitate was dissolved in 10 mL TFA and stirred at room temperature for 15 minutes, then the mixture was poured into ice water. The resultant precipitate was collected, dissolved in dichloromethane, dried over MgSO4, filtered and evaporated to give the crude benzyl 4-amino-2-oxo-1,2-dihydroquinoline-3-carboxylate (600 mg) which was used as this without further purification. MS 295 (MH+).

後処理

  1. temperaturecooled to room temperature
  2. customThe resultant precipitate was collected
  3. dissolutiondissolved in dichloromethane
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-da3d3555ab9f4185bd40e31d934fa216
出典データセット
uspto-grants-2011_04
特許番号
US07928111B2

反応ノート

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