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Morpholine → HCID 86685989、化合物

HRID 2277692
ノート
印刷プレビュー

反応式

HRID 2277692 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[N:7]([C:13]1[CH:14]=[C:15]([CH2:19][C:20](O)=[O:21])[CH:16]=[N:17][CH:18]=1)[CH2:6][CH2:5]2.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC.[NH:54]1[CH2:59][CH2:58][O:57][CH2:56][CH2:55]1>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[N:7]([C:13]1[CH:18]=[N:17][CH:16]=[C:15]([CH2:19][C:20]([N:54]3[CH2:59][CH2:58][O:57][CH2:56][CH2:55]3)=[O:21])[CH:14]=1)[CH2:6][CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8083MorpholineHCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86685988HCID 86685988、化合物

生成物 1

HCID 86685989HCID 86685989、化合物収率 13.9%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

[5-(6-Chloro-1-oxo-3,4-dihydro-1H-isoquinolin-2-yl)-pyridin-3-yl]-acetic acid (50 mg, 0.16 mmol), HATU (122 mg, 0.32 mmol), Et3N (64 mg, 0.64 mmol) and morpholine (56 mg, 0.64 mmol) were dissolved in DCM (4.0 mL) and the resulting reaction mixture was stirred at room temperature overnight. After evaporating off the DCM, the residue was re-dissolved in EtOAc and was washed with brine. The organic layer was dried over anhy. Na2SO4, filtered and concentrated in vacuo to give a crude product which was then purified by prep-HPLC to give the title compound (8.5 mg, 13.9%) as light yellow oil. MS: 386.1 (M+H+).

後処理

  1. customthe resulting reaction mixture
  2. customAfter evaporating off the DCM
  3. dissolutionthe residue was re-dissolved in EtOAc
  4. washwas washed with brine
  5. customThe organic layer was dried over anhy
  6. filtrationNa2SO4, filtered
  7. concentrationconcentrated in vacuo
  8. customto give a crude product which
  9. customwas then purified by prep-HPLC

出典と根拠

ORDレコード
ord-1d4d64587d254ca392f3dd43caabd3bf
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133158B2

反応ノート

読み込み中…

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