Sodium Carbonate → HCID 21697868, 화합물

HRID 379082

반응식

HRID 379082 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 21697868HCID 21697868, 화합물

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2fb5417e2cc842c6ac1694a12d2490dc
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297282B1

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