Triethylamine → HCID 71255527、化合物

HRID 540166ノート

反応式

HRID 540166 の反応式
[O:1]=[S:2]1(=[O:25])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][N:5]([C:13]2[CH:22]=[C:21]([NH2:23])[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([CH3:24])[CH:19]=3)[N:14]=2)[CH2:4][CH2:3]1.C(N(CC)CC)C.[Br:33][C:34]([CH3:39])([CH3:38])[C:35](Cl)=[O:36]>C(Cl)(Cl)Cl>[Br:33][C:34]([CH3:39])([CH3:38])[C:35]([NH:23][C:21]1[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([CH3:24])[CH:19]=2)[N:14]=[C:13]([N:5]2[CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[S:2](=[O:1])(=[O:25])[CH2:3][CH2:4]2)[CH:22]=1)=[O:36]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 111060492-Bromo-2-methylpropanoyl chlorideHCID 712554832-(1,1-Dioxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylquinolin-4-amine

生成物 1

HCID 71255527HCID 71255527、化合物収率 63.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
110 °C

実験手順

To a solution of 2-(1,1-dioxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylquinolin-4-amine (200 mg, 0.566 mmol) in chloroform (10 mL) was added triethylamine (0.124 mL), followed by 2-bromo-2-methylpropionyl chloride (286 mg, 1.30 mmol). The resulting mixture was heated at 110° C. for 2 hours under microwave irradiation. After being cooled to room temperature, the mixture was concentrated in vacuo. The residue was diluted with ethyl acetate (35 mL), washed with brine and dried over sodium sulfate, and concentrated in vacuo. The residue was purified by flash chromatography to afford 180 mg of the title compound as a light solid (yield was 63%).

後処理

  1. temperatureAfter being cooled to room temperature
  2. concentrationthe mixture was concentrated in vacuo
  3. additionThe residue was diluted with ethyl acetate (35 mL)
  4. washwashed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-b044e258d0774458bd65a8fe2d5f6897
出典データセット
uspto-grants-2014_10
特許番号
US08871756B2

反応ノート

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