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p-Toluenesulfonic acid → HCID 67696440、化合物

HRID 1609392
ノート
印刷プレビュー

反応式

HRID 1609392 の反応式
[C:1](Cl)(=O)[C:2](Cl)=[O:3].[C:7]([O:10][CH2:11][CH:12]1[CH2:24][CH2:23][N:15]2[C:16]3[C:21]([CH:22]=[C:14]2[CH2:13]1)=[CH:20][CH:19]=[CH:18][CH:17]=3)(=[O:9])[CH3:8].C(N(CC)CC)C.Cl.[NH:33]1[C:41]2[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=2)[C:35]([CH2:42][C:43](=[NH:48])[O:44]C(C)C)=[CH:34]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl.C1(C)C=CC=CC=1>[C:7]([O:10][CH2:11][CH:12]1[CH2:24][CH2:23][N:15]2[C:16]3[C:21]([C:22]([C:1]4[C:2](=[O:3])[NH:44][C:43](=[O:48])[C:42]=4[C:35]4[C:36]5[C:41](=[CH:40][CH:39]=[CH:38][CH:37]=5)[NH:33][CH:34]=4)=[C:14]2[CH2:13]1)=[CH:20][CH:19]=[CH:18][CH:17]=3)(=[O:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6101p-Toluenesulfonic acidHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 14954045HCID 14954045、化合物HCID 20084644HCID 20084644、化合物

生成物 1

HCID 67696440HCID 67696440、化合物収率 38%

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 6344Dichloromethane溶媒

実験手順

165 mg (1.38 mmol) of oxalyl chloride were added to a stirred solution of 300 mg (1.24 mmol) of 8-acetoxymethyl-6,7,8,9-tetrahydropyrido[1,2-a]indole in 50 ml of dichloromethane at 0° C. The resulting solution was stirred for 15 minutes and the solvent was removed by evaporation. The residue was dissolved in 30 ml of toluene and added dropwise to a stirred solution of 496 mg (4.96 mmol) of triethylamine and mg (1.31 mmol) of isopropyl 3-indoleacetimidate hydrochloride in 20 ml of toluene. After 18 hours, 1.16 g (6.2 mmol) of p-toluenesulfonic acid were added and stirring was continued for 1 hour. The mixture was then partitioned between dichloromethane and water. The organic phase was dried over sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography on silica gel using ethyl acetate/petroleum ether (1:1) for the elution to give 170 mg (38%) of 3-[8-(acetoxymethyl) -6,7,8,9-tetrahydropyrido[1,2-a]indol-10-yl]-4-[3-indolyl)-1H-pyrrole-2,5-dione in the form of an orange colored solid of melting point 264°-265° C.

後処理

  1. customthe solvent was removed by evaporation
  2. dissolutionThe residue was dissolved in 30 ml of toluene
  3. waitAfter 18 hours
  4. stirringstirring
  5. waitwas continued for 1 hour
  6. customThe mixture was then partitioned between dichloromethane and water
  7. dry with materialThe organic phase was dried over sodium sulfate
  8. customevaporated to dryness
  9. customThe residue was purified by flash chromatography on silica gel
  10. washfor the elution

出典と根拠

ORDレコード
ord-1f6073b1febc44cd89158fd842ee643b
出典データセット
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05399712

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート