Diisopropylethylamine → HCID 67450427、化合物

HRID 2368084ノート

反応式

HRID 2368084 の反応式
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

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 234412462-Chloro-1,3-benzoxazol-6-OLHCID 67449164HCID 67449164、化合物

生成物 1

HCID 67450427HCID 67450427、化合物収率 77%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-4e66ce45b31b4c8cbaa8a3c91d15f9ec
出典データセット
uspto-grants-2014_04
特許番号
US08703758B2

反応ノート

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