Sodium Carbonate → HCID 58624190、化合物

HRID 349502

反応式

HRID 349502 の反応式
[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([NH:12][C:13](=[NH:23])[C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[CH:5]=1.[O-]Cl.[Na+].C([O-])([O-])=O.[Na+].[Na+]>CO>[CH3:1][O:2][C:3]([C:4]1[C:5]2[N:23]=[C:13]([C:14]3[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=3)[NH:12][C:6]=2[C:7]([O:10][CH3:11])=[CH:8][CH:9]=1)=[O:24]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 23665760Sodium HypochloriteHCID 178498286HCID 178498286、化合物

生成物 1

HCID 58624190HCID 58624190、化合物収率 46.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-[(4-nitro-benzimidoyl)-amino]-4-methoxy-benzoic acid methyl ester (1.63 g, 4.95 mmol) was dissolved in 50% methanol, and 5% NaOCl was added dropwise thereto at room temperature. After checking the reaction by TLC, Na2CO3 (1.05 g, 9.38 mmol) seas added dropwise thereto and refluxed for 40 min. The resulting solution was cooled to room temperature, extracted with ethyl acetate and the extract was concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (0.75 g, 2.28 mmol) in a yield of 46%.

後処理

  1. customat room temperature
  2. additionadded dropwise
  3. temperaturerefluxed for 40 min
  4. extractionextracted with ethyl acetate
  5. concentrationthe extract was concentrated under a reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f504fecf8c0247e4ae3d761ac9265e77
出典データセット
uspto-grants-2007_02
特許番号
US07179832B2

関連ノート

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