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Phosphorus pentachloride → HCID 12783772、化合物

HRID 1701517
ノート
印刷プレビュー

反応式

HRID 1701517 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 12783772HCID 12783772、化合物収率 50%

試薬・触媒・溶媒 1

HCID 11
1,2-Dichloroethane
溶媒

実験手順

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%.

後処理

  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)

出典と根拠

ORDレコード
ord-125fb7b7af0f4d3fbd21a82792a6316c
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04194003

反応ノート

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