Triethylamine → HCID 58629071、化合物

HRID 1678048ノート

反応式

HRID 1678048 の反応式
Cl[C:2]1[C:3]2[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[S:8][C:4]=2[N:5]=[CH:6][N:7]=1.Cl.[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([CH:23]([NH2:25])[CH3:24])=[CH:19][CH:18]=1.C(N(CC)CC)C>CN(C=O)C.O>[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([CH:23]([NH:25][C:2]2[C:3]3[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[S:8][C:4]=3[N:5]=[CH:6][N:7]=2)[CH3:24])=[CH:19][CH:18]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 122252624-Chloro-6-nitrothieno(2,3-d)pyrimidineHCID 17938752HCID 17938752、化合物

生成物 1

HCID 58629071HCID 58629071、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4-chloro-6-nitrothieno[2,3-d]pyrimidine (prepared as disclosed in Bull. Chim. Soc. Fr. 1975, 3-4, Pt. 2, 592) (500 mg, 2.3 mmol), 1-(4-methoxyphenyl)ethanamine HCl (513 mg, 2.8 mmol), and triethylamine (581 mg, 5.7 mmol) in DMF (7 mL) was allowed to react for 24 hours at 20° C. The reaction mixture was diluted with water and extracted thrice into Et2O. The organic portions were combined, washed with brine, and dried (Na2SO4). The mixture was filtered through silica gel, and the solvent was removed in vacuo. The residue was purified by flash chromatography (40 percent EtOAc in pentane), yielding 385 mg.

後処理

  1. customto react for 24 hours at 20° C
  2. extractionextracted thrice into Et2O
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationThe mixture was filtered through silica gel
  6. customthe solvent was removed in vacuo
  7. customThe residue was purified by flash chromatography (40 percent EtOAc in pentane)
  8. customyielding 385 mg

出典と根拠

ORDレコード
ord-868f58824ea64c278a1c9a23750d7c16
出典データセット
uspto-grants-2011_08
特許番号
US08008487B2

反応ノート

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