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Chloroform → HCID 22137207, 화합물

HRID 1827299
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HRID 1827299 반응식
[S:1]([Cl:5])(=[O:4])(=[O:3])O.C(Cl)Cl.[C:9]1([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:17][CH:16]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(Cl)(Cl)Cl>[Cl-].[Na+].O>[Cl:5][S:1]([C:12]1[CH:11]=[CH:10][C:9]([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:22]=[CH:23][C:24]([S:1]([Cl:5])(=[O:4])=[O:3])=[CH:25][CH:26]=3)=[CH:17][CH:16]=2)=[CH:14][CH:13]=1)(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 6344DichloromethaneHCID 7115p-TerphenylHCID 24638Chlorosulfonic acid3회

생성물 1

HCID 22137207HCID 22137207, 화합물수율 67%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

실험 절차

Under the nitrogen gas atmosphere, chloro sulfuric acid is diluted by adding chloro sulfuric acid (0.53 ml, 8 eq.) into methylene chloride (10 ml), and 1,1′:4′,1″-terphenyl (0.230 g, 1.0 mmol) is added gradually into a container in which diluted chloro sulfuric acid is contained keeping the temperature at 0° C., then stirred at the room temperature for 6 hours. The obtained reacted mixture is poured into brine, and deposited white insoluble is removed by suction filtration. Since the small amount of product is possible to be remained, the residue is washed well by methylene chloride. Then, this solution and the extracted solution are dried up using magnesium sulfate. Solvent is vaporized off under the vacuum condition, and the impurity is removed from the obtained crude product by isolating by a column chromatography (φ=50 mm, h=100 mm; CHCl3). Thus, 4,4″-dichlorosulfonyl1,1′:4′,1″-terphenyl (0.288 g, 0.67 mmol, 67%) is obtained as a colorless crystal (compound F).

후처리

  1. customat 0° C.
  2. customThe obtained reacted mixture
  3. customdeposited white insoluble is removed by suction filtration
  4. washthe residue is washed well by methylene chloride
  5. customThen, this solution and the extracted solution are dried up
  6. customthe impurity is removed from the
  7. customobtained crude product

출처 및 근거

ORD 기록
ord-8e895a45e1394778ba92dc52382a4f9d
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07053173B2

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