Triethylamine → HCID 58629071, 화합물

HRID 1678048노트

반응식

HRID 1678048 반응식
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

참가 물질

6

반응물 3

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

생성물 1

HCID 58629071HCID 58629071, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-868f58824ea64c278a1c9a23750d7c16
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08008487B2

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