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Sodium Iodide → HCID 14727018、化合物

HRID 329409
ノート
印刷プレビュー

反応式

HRID 329409 の反応式
Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:13]=[N:14][S:15][CH:16]=2)=[CH:8][CH:7]=1.[S:17]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)=[N:18]1.C(N(C(C)C)CC)(C)C.C(=O)([O-])[O-].[Na+].[Na+].[I-].[Na+]>C(OCC)(=O)C.CC(CC(C)C)=O>[S:17]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[C:19]([N:26]2[CH2:27][CH2:28][N:29]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]3[CH:11]=[CH:10][C:9]([C:12]4[N:13]=[N:14][S:15][CH:16]=4)=[CH:8][CH:7]=3)[CH2:30][CH2:31]2)=[N:18]1
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 5238Sodium IodideHCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 27721443-(1-Piperazinyl)-1,2-benzisothiazoleHCID 19872068HCID 19872068、化合物

生成物 1

HCID 14727018HCID 14727018、化合物

試薬・触媒・溶媒 2

HCID 7909
Methyl Isobutyl Ketone
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a 65 ml round-bottom flask equipped with condenser and N2 inlet were added 1.43 g (5.66 mmol) 4-(4-(4-chlorobutyl)phenyl)-1,2,3-thiadiazole, 0.90 g (4.11 mmol) N-benzisothiazolylpiperazine, 1.43 ml (8.22 mmol)diisopropylethyl amine, 0.87 g (8.22 mmol) sodium carbonate, 2 mg sodium iodide, and 30 ml methylisobutyl ketone. The reaction was refluxed for 24 hours, cooled, filtered, and the filtrate evaporated. The residue was chromatographed on silica gel using ethyl acetate/methylene chloride as eluent to give an oil, which was taken up in ethyl acetate and precipitated by addition of ethyl acetate saturated with HCl. The solid was filtered, washed with ethyl acetate, and dried to afford 1.70 g (87.6%), m.p. 246°-247° C., white solid.

後処理

  1. customTo a 65 ml round-bottom flask equipped with condenser and N2 inlet
  2. temperatureThe reaction was refluxed for 24 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. customthe filtrate evaporated
  6. customThe residue was chromatographed on silica gel
  7. customto give an oil, which
  8. customprecipitated by addition of ethyl acetate saturated with HCl
  9. filtrationThe solid was filtered
  10. washwashed with ethyl acetate
  11. customdried
  12. customto afford 1.70 g (87.6%), m.p. 246°-247° C., white solid

出典と根拠

ORDレコード
ord-e8b3066c1cf1453fb3130675194718b1
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04891375

反応ノート

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