Hydrochloric Acid → HCID 54511686、化合物

HRID 1387530ノート

反応式

HRID 1387530 の反応式
Cl.[CH3:2][O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([N:13](C(=O)C)[C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)[CH:6]=1>O1CCCC1.CO>[CH3:2][O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[C:7]([NH:13][C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[C:16]([Cl:21])[CH:15]=2)[CH:6]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 543001583-[Acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester

生成物 1

HCID 54511686HCID 54511686、化合物収率 23.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Concentrated HCl (45 mL) was added to a solution of 3-[acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester (11.46 g, 31.12 mmol) in a mixture of tetrahydrofuran (75 mL) and methanol (75 mL). The reaction was heated to reflux. After 3 days, the solvent was removed in vacuo and the residue was dissolved in ethyl acetate and dried (MgSO4). The ethyl acetate was removed under reduced pressure to give the product (2.4 g); m.p. 134-135° C. after chromatography on silica gel in ethyl acetate followed by recrystallization from ether/hexane 1:9.

後処理

  1. temperatureThe reaction was heated to reflux
  2. customthe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. dry with materialdried (MgSO4)
  5. customThe ethyl acetate was removed under reduced pressure

出典と根拠

ORDレコード
ord-82a32adeb35345acbbd2ecd0eefd25fa
出典データセット
uspto-grants-2001_07
特許番号
US06268387B1

反応ノート

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