Piperidinium acetate → HCID 178451231、化合物

HRID 1620609ノート

反応式

HRID 1620609 の反応式
[O:1]=[C:2]1[N:6]=[C:5]([NH:7][CH2:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4][S:3]1.[F:16][C:17]([F:38])([F:37])[C:18]1[CH:32]=[C:31]([C:33]([F:36])([F:35])[F:34])[CH:30]=[CH:29][C:19]=1[CH2:20][N:21]1[CH2:26][CH2:25][CH:24]([CH:27]=O)[CH2:23][CH2:22]1.C([O-])(=O)C.[NH2+]1CCCCC1>CC(O)C>[F:38][C:17]([F:16])([F:37])[C:18]1[CH:32]=[C:31]([C:33]([F:36])([F:35])[F:34])[CH:30]=[CH:29][C:19]=1[CH2:20][N:21]1[CH2:26][CH2:25][CH:24](/[CH:27]=[C:4]2/[C:5]([NH:7][CH2:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])=[N:6][C:2](=[O:1])[S:3]/2)[CH2:23][CH2:22]1

参加物

5

反応物 3

HCID 3014295Piperidinium acetateHCID 866786631-[2,4-Bis(trifluoromethyl)benzyl]piperidine-4-carbaldehydeHCID 178451230HCID 178451230、化合物

生成物 1

HCID 178451231HCID 178451231、化合物収率 64.6%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
70 °C

実験手順

To a solution of tert-butyl N-(2-oxo-2,5-dihydro-1,3-thiazol-4-yl)glycinate (4.41 g) and 1-[2,4-bis(trifluoromethyl)benzyl]piperidine-4-carbaldehyde (5.00 g) in 2-propanol (50 mL) was added piperidinium acetate (2.14 g). The reaction mixture was stirred at 70° C. for 3 hr and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) and recrystallized from ethyl acetate/heptane to give the title compound (5.25 g).

後処理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  3. customrecrystallized from ethyl acetate/heptane

出典と根拠

ORDレコード
ord-0f630f07531f46c898fa20a0433f1ad0
出典データセット
uspto-grants-2014_07
特許番号
US08772277B2

反応ノート

読み込み中…