Potassium Carbonate → HCID 86631471、化合物

HRID 1806023ノート

反応式

HRID 1806023 の反応式
C([NH:9][C:10](=[S:32])[NH:11][C:12]1[C:17]([O:18][C:19]2[CH:20]=[C:21]([CH:27]=[CH:28][C:29]=2[Cl:30])[C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:16][C:15]([Br:31])=[CH:14][N:13]=1)(=O)C1C=CC=CC=1.C([O-])([O-])=O.[K+].[K+]>C(O)C>[Br:31][C:15]1[CH:16]=[C:17]([O:18][C:19]2[CH:20]=[C:21]([CH:27]=[CH:28][C:29]=2[Cl:30])[C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:12]([NH:11][C:10]([NH2:9])=[S:32])=[N:13][CH:14]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 86631470HCID 86631470、化合物

生成物 1

HCID 86631471HCID 86631471、化合物収率 26.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 3-(2-(3-benzoylthioureido)-5-bromopyridin-3-yloxy)-4-chlorobenzoate (8.05 g, 15.1 mmol) and K2CO3 (10.4 g, 75.3 mmol) were placed in ethanol (150 mL) and heated to reflux for 2 days and then cooled. The reaction mixture was filtered and the filtrate was concentrated, triturated with water, and dried. The remaining solid was dissolved in CH2Cl2 and purified by silica gel chromatography to give ethyl 3-(5-bromo-2-thioureidopyridin-3-yloxy)-4-chlorobenzoate (1.70 g, 26.2% yield).

後処理

  1. temperatureheated
  2. temperatureto reflux for 2 days
  3. temperaturecooled
  4. filtrationThe reaction mixture was filtered
  5. concentrationthe filtrate was concentrated
  6. customtriturated with water
  7. customdried
  8. dissolutionThe remaining solid was dissolved in CH2Cl2
  9. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-add7393513814522b480e2bb033adfe2
出典データセット
uspto-grants-2013_01
特許番号
US08354540B2

反応ノート

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