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Phosphorus pentachloride → HCID 68296403, 화합물

HRID 631871
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HRID 631871 반응식
[C:1]1([S:7]([NH:10][C:11]2[CH:20]=[CH:19][C:18]3[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[C:12]=2[C:21]([NH2:23])=O)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)(Cl)Cl.C(=O)([O-])O.[Na+]>C(Cl)Cl>[C:21]([C:12]1[C:13]2[CH2:14][CH2:15][CH2:16][CH2:17][C:18]=2[CH:19]=[CH:20][C:11]=1[NH:10][S:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:8])=[O:9])#[N:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24819Phosphorus pentachlorideHCID 516892Sodium BicarbonateHCID 68296406HCID 68296406, 화합물2회

생성물 1

HCID 68296403HCID 68296403, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Benzenesulfonylamino-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid amide (Intermediate 2, 1.2 g) was dissolved in dry DCM (20 mL) and phosphorous pentachloride (0.9 g) was added. The mixture was stirred for 3 hours then saturated aqueous sodium hydrogencarbonate was added carefully and the products were extracted into ethyl acetate. The organic solution was dried with magnesium sulfate, filtered and the solvent was removed by evaporation. The residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane. The fractions containing the desired product were combined and the solvent was evaporated to give the title compound as an off-white solid.

후처리

  1. extractionthe products were extracted into ethyl acetate
  2. dry with materialThe organic solution was dried with magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent was removed by evaporation
  5. customThe residue was purified by chromatography on silica
  6. washeluting with a mixture of ethyl acetate and cyclohexane
  7. additionThe fractions containing the desired product
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-61610417cac24ead97a9e22b89bd09e1
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321740B2

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