Sodium Carbonate → HCID 69131964、化合物

HRID 349497

反応式

HRID 349497 の反応式
[CH3:1][O:2][C:3](=[O:23])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([NH:12][C:13](=[NH:22])[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[C:16]([Cl:21])[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:22]=[C:13]([C:14]3[CH:19]=[CH:18][C:17]([F:20])=[C:16]([Cl:21])[CH:15]=3)[NH:12][C:6]=2[C:7]([O:10][CH3:11])=[CH:8][CH:9]=1)=[O:23]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 23665760Sodium HypochloriteHCID 178498285HCID 178498285、化合物

生成物 1

HCID 69131964HCID 69131964、化合物収率 30%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-[(3-chloro-4-fluoro-benzimidoyl)-amino]-4-methoxy-benzoic acid methyl ester (3.24 g, 9.62 mmol) was dissolved in 50% methanol and 5% NaOCl (18 ml, 11.90 mmol) was added dropwise thereto at room temperature. After 5 min, Na2CO3 (2.04 g, 19.25 mmol) was added dropwise thereto and refluxed for 5 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 (0.95 g, 2.83 mmol) in a yield of 30%.

後処理

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

出典と根拠

ORDレコード
ord-ff4cd207c0da4cfb940b83506bb49d46
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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