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Phosphorus pentachloride → HCID 12783772, 화합물

HRID 1701517
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HRID 1701517 반응식
[CH3:1][O:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([C:13](Cl)=[O:14])=[CH:5][CH:4]=1.P(Cl)(Cl)(Cl)(Cl)Cl.[CH3:22][N:23]1[CH:27]=[CH:26][CH:25]=[C:24]1[C:28]([O:30][CH3:31])=[O:29].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[CH3:22][N:23]1[CH:27]=[C:26]([C:13]([C:6]2[C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[O:14])[CH:25]=[C:24]1[C:28]([O:30][CH3:31])=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 24819Phosphorus pentachlorideHCID 142178Methyl 1-methylpyrrole-2-carboxylateHCID 6451240Aluminum(III) ChlorideHCID 114586874-Methoxy-1-naphthoyl Chloride

생성물 1

HCID 12783772HCID 12783772, 화합물수율 50%

시약·촉매·용매 1

HCID 11
1,2-Dichloroethane
용매

실험 절차

4-Methoxy-naphthoic acid chloride (35 g; prepared by action of phosphorous pentachloride on the acid of m.p. 250° C.) followed by methyl 1-methyl-pyrrole-2-carboxylate (22 g) are dissolved in 1,2-dichloroethane (400 ml). To the stirred solution, at about -20° C., is slowly added anhydrous aluminium chloride (23 g). After one hour, the resulting material is poured over 1 kg crushed ice. The organic phase is decanted off and the aqueous phase is extracted with chloroform (500 ml). The organic solution is then dried and the solvents are evaporated off. The solid residue (28 g) is washed with isopropyl ether (200 ml), to give methyl 1-methyl-4-(4-methoxy-1-naphthoyl)-pyrrole-2-carboxylate, m.p.=162° C., in a yield of 50%.

후처리

  1. customat about -20° C.
  2. additionthe resulting material is poured over 1 kg
  3. customcrushed ice
  4. customThe organic phase is decanted off
  5. extractionthe aqueous phase is extracted with chloroform (500 ml)
  6. customThe organic solution is then dried
  7. customthe solvents are evaporated off
  8. washThe solid residue (28 g) is washed with isopropyl ether (200 ml)

출처 및 근거

ORD 기록
ord-125fb7b7af0f4d3fbd21a82792a6316c
출처 데이터셋
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04194003

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