Diisopropylethylamine → HCID 67343276、化合物

HRID 451412

反応式

HRID 451412 の反応式
[C:1]([N:8]1CCC(N)C[CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].Cl[C:16]1[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18][N:17]=1.C([N:26]([CH2:30][CH3:31])[CH:27]([CH3:29])C)(C)C>O1CCOCC1.O>[C:4]([O:3][C:1](=[O:2])[NH:8][CH:9]1[CH2:29][CH2:27][N:26]([C:16]2[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18][N:17]=2)[CH2:30][CH2:31]1)([CH3:7])([CH3:6])[CH3:5]

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 5817964-Chloro-6-methylpyrimidineHCID 12682914-Amino-1-Boc-piperidine

生成物 1

HCID 67343276HCID 67343276、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
150 °C

実験手順

A suspension of Boc-4-aminopiperidine (613 mg, 3 mmol), 4-chloro-6-methylpyrimidine (433 mg, 3.3 mmol) and N,N-diisopropylethyl amine (771 L, 4.5 mmol) in dioxane (12 mL) was heated to 150° C. in the microwave for 30 minutes. The reaction was diluted with water and extracted twice with ethyl acetate. The combined organic layers were washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel using a gradient from AcOEt to AcOEt/EtOH 9:1 as eluent. The title compound was obtained as a light yellow solid (693 mg, 79%).

後処理

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organic layers were washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product was purified by column chromatography on silica gel using a gradient from AcOEt to AcOEt/EtOH 9:1 as eluent

出典と根拠

ORDレコード
ord-6de883d95cf14582bc0237df04c0840d
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

関連ノート

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