Triethylamine → HCID 71255527, 화합물

HRID 540166노트

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HRID 540166 반응식
[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]

참가 물질

5

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

생성물 1

HCID 71255527HCID 71255527, 화합물수율 63.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
110 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b044e258d0774458bd65a8fe2d5f6897
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871756B2

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