Dicyclohexylcarbodiimide → HCID 178477423、化合物

HRID 1682160ノート

反応式

HRID 1682160 の反応式
[Cl:1][C:2]1[C:10]([CH2:11][S:12][CH2:13][CH3:14])=[C:9]([S:15]([CH3:18])(=[O:17])=[O:16])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.C(=O)([O-])[O-].[K+].[K+].C1(N=C=NC2CCCCC2)CCCCC1.[CH2:40]([N:42]1[C:46](=[O:47])[CH:45]=[CH:44][NH:43]1)[CH3:41]>C(O)(CC)(C)C>[Cl:1][C:2]1[C:10]([CH2:11][S:12][CH2:13][CH3:14])=[C:9]([S:15]([CH3:18])(=[O:17])=[O:16])[CH:8]=[CH:7][C:3]=1[C:4]([C:45]1[CH:44]=[N:43][N:42]([CH2:40][CH3:41])[C:46]=1[OH:47])=[O:6]

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 11430Potassium CarbonateHCID 103131081-ethyl-1H-pyrazol-5-olHCID 151328402-Chloro-3-ethylthiomethyl-4-methanesulfonylbenzoic acid

生成物 1

HCID 178477423HCID 178477423、化合物

試薬・触媒・溶媒 1

HCID 64052-Methyl-2-butanol溶媒2 回

実験手順

3 g of 2-chloro-3-ethylthiomethyl-4-methanesulfonylbenzoic acid, 0.72 g of potassium carbonate, 50 ml of t-amyl alcohol, 1.95 g of N,N'-dicyclohexylcarbodiimide and 4.5 g of a 25% t-amyl alcohol solution of 1-ethyl-5-pyrazolone were mixed and heated under stirring for 4 hours at a temperature of from 70° to 80° C. After cooling, the mixture was distilled under reduced pressure, and 200 ml of water was added to the residue. After filtering off the insolubles, the filtrate was washed with chloroform. Hydrochloric acid was added to the aqueous layer, and the mixture was extracted with chloroform. The extract was dried, and the solvent was distilled off to obtain the desired product as a crude product. The crude product was recrystallized from ethanol to obtain 1.88 g of the purified product. (Melting point: 142°-145° C.)

後処理

  1. temperatureheated
  2. temperatureAfter cooling
  3. distillationthe mixture was distilled under reduced pressure, and 200 ml of water
  4. additionwas added to the residue
  5. filtrationAfter filtering off the insolubles
  6. washthe filtrate was washed with chloroform
  7. additionHydrochloric acid was added to the aqueous layer
  8. extractionthe mixture was extracted with chloroform
  9. customThe extract was dried
  10. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-57eb9c13ad064721a7e11a349e3f304f
出典データセット
uspto-grants-1992_12
特許番号
US05175299

反応ノート

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