Sodium Carbonate → HCID 21697868、化合物

HRID 379082

反応式

HRID 379082 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[C:9]=1Cl.[Cl:18][C:19]1[CH:24]=[C:23]([Cl:25])[CH:22]=[CH:21][C:20]=1[SH:26]>C1(C)C(C)=CC=CC=1>[Cl:7][C:8]1[C:9]([S:26][C:20]2[CH:21]=[CH:22][C:23]([Cl:25])=[CH:24][C:19]=2[Cl:18])=[C:10]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 185552,3-DichloronitrobenzeneHCID 707302,4-Dichlorobenzenethiol

生成物 1

HCID 21697868HCID 21697868、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

Sodium carbonate (13.8 g) is added to a solution of 1,2-dichloro-3-nitrobenzene (19.29 g) and 2,4-dichlorothio-phenol (17.9 g) in xylene (250 ml), and the resulting mixture is heated for 5 hours at reflux temperature. The precipitate is separated by filtration, washed with xylene and the combined organic phases are concentrated. The resultant residue is mixed with petroleum ether and stirred for 1 hour at room temperature. Following this, the crystalline material is suction filtered and washed with petroleum ether, and any remaining solvent is removed in a vacuum. Yield: 25.6 g of colourless crystals (76.6%).

後処理

  1. temperaturethe resulting mixture is heated for 5 hours
  2. temperatureat reflux temperature
  3. customThe precipitate is separated by filtration
  4. washwashed with xylene
  5. concentrationthe combined organic phases are concentrated
  6. additionThe resultant residue is mixed with petroleum ether
  7. filtrationfiltered
  8. washwashed with petroleum ether
  9. customany remaining solvent is removed in a vacuum

出典と根拠

ORDレコード
ord-2fb5417e2cc842c6ac1694a12d2490dc
出典データセット
uspto-grants-2001_10
特許番号
US06297282B1

関連ノート

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