Diisopropylethylamine → HCID 67450427, 화합물

HRID 2368084노트

반응식

HRID 2368084 반응식
Cl.[CH3:2][CH:3]([NH:12][C:13](=[O:15])[CH3:14])[CH2:4][CH2:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.Cl[C:17]1[O:18][C:19]2[CH:25]=[C:24]([OH:26])[CH:23]=[CH:22][C:20]=2[N:21]=1.C(N(CC)C(C)C)(C)C>CN(C=O)C>[OH:26][C:24]1[CH:23]=[CH:22][C:20]2[N:21]=[C:17]([N:9]3[CH2:8][CH2:7][CH:6]([CH2:5][CH2:4][CH:3]([NH:12][C:13](=[O:15])[CH3:14])[CH3:2])[CH2:11][CH2:10]3)[O:18][C:19]=2[CH:25]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 234412462-Chloro-1,3-benzoxazol-6-OLHCID 67449164HCID 67449164, 화합물

생성물 1

HCID 67450427HCID 67450427, 화합물수율 77%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of N-[1-methyl-3-(piperidin-4-yl)propyl]acetamide hydrochloride (500 mg), 2-chloro-1,3-benzoxazol-6-ol (361 mg) and N,N-diisopropylethylamine (826 mg) in DMF (15 mL) was stirred at 100° C. for 10 hr. The reaction mixture was allowed to cool, and the solvent was evaporated under reduced pressure. The residue was diluted with ethyl acetate/THF mixed solvent (10/1), and the solution was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (543 mg).

후처리

  1. temperatureto cool
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was diluted with ethyl acetate/THF mixed solvent (10/1)
  4. washthe solution was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-4e66ce45b31b4c8cbaa8a3c91d15f9ec
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703758B2

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