Methanol → HCID 71255101、化合物

HRID 540171ノート

反応式

HRID 540171 の反応式
Br[C:2]([CH3:31])([CH3:30])[C:3]([NH:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([CH3:16])[CH:14]=2)[N:9]=[C:8]([N:17]2[CH2:23][C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[S:20](=[O:29])(=[O:28])[CH2:19][CH2:18]2)[CH:7]=1)=[O:4].C(N)C.[CH3:35][OH:36]>>[O:28]=[S:20]1(=[O:29])[C:21]2[CH:27]=[CH:26][CH:25]=[CH:24][C:22]=2[CH2:23][N:17]([C:8]2[CH:7]=[C:6]([NH:5][C:3](=[O:4])[C:2]([O:36][CH3:35])([CH3:31])[CH3:30])[C:15]3[C:10](=[CH:11][CH:12]=[C:13]([CH3:16])[CH:14]=3)[N:9]=2)[CH2:18][CH2:19]1

参加物

4

反応物 3

HCID 887MethanolHCID 6341EthylamineHCID 71255527HCID 71255527、化合物

生成物 1

HCID 71255101HCID 71255101、化合物

実験手順

To a solution of 2-bromo-N-[2-(1,1-dioxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylquinolin-4-yl]-2-methylpropanamide (80 mg, 0.159 mmol, prepared in Example 40-2) in methanol (5 mL) was added ethylamine (1 mL), the resulting mixture was heated under reflux overnight. After being cooled to room temperature, the resulting mixture was concentrated in vacuo. The residue was purified by preparative TLC (eluting with 33% ethyl acetate in hexanes) to afford 15 mg of the title compound as a light powder (yield was 21%). MS obsd. (ESI+) [(M+H)+] 454, 1H NMR (400 MHz, CD3OD) δ ppm 7.94-7.89 (m, 3 H), 7.58 (m, 2 H), 7.43-7.39 (m, 3 H), 5.17 (s, 2 H), 4.50 (brs, 2 H), 3.59 (m, 2 H), 3.50 (s, 3 H), 2.46 (s, 3 H), 1.56 (s, 6 H).

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux overnight
  3. concentrationthe resulting mixture was concentrated in vacuo
  4. customThe residue was purified by preparative TLC (eluting with 33% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-6c1520ce02c140b684a6cea3ccfe39b7
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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