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Dichloromethane → N-(3-((R)-3-((S)-1-(4-bromophenyl)ethyl)-2-oxo-6-phenyl-1,3-oxazinan-6-yl)propyl)-N-methylacetamide

HRID 1191731
ノート
印刷プレビュー

反応式

HRID 1191731 の反応式
CS(OC[CH2:7][CH2:8][C@@:9]1([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[O:14][C:13](=[O:15])[N:12]([C@H:16]([C:18]2[CH:23]=[CH:22][C:21]([Br:24])=[CH:20][CH:19]=2)[CH3:17])[CH2:11][CH2:10]1)(=O)=O.[H-].[Na+].[CH3:33][NH:34][C:35](=[O:37])[CH3:36].[CH2:38](Cl)Cl>>[Br:24][C:21]1[CH:20]=[CH:19][C:18]([C@@H:16]([N:12]2[CH2:11][CH2:10][C@:9]([CH2:8][CH2:7][CH2:33][N:34]([CH3:38])[C:35](=[O:37])[CH3:36])([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[O:14][C:13]2=[O:15])[CH3:17])=[CH:23][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 6582N-MethylacetamideHCID 24758Sodium hydrideHCID 596357093-((R)-3-((S)-1-(4-bromophenyl)ethyl)-2-oxo-6-phenyl-1,3-oxazinan-6-yl)propyl methanesulfonate

生成物 1

HCID 59635812N-(3-((R)-3-((S)-1-(4-bromophenyl)ethyl)-2-oxo-6-phenyl-1,3-oxazinan-6-yl)propyl)-N-methylacetamide収率 68%

実験手順

To a solution of 3-((R)-3-((S)-1-(4-bromophenyl)ethyl)-2-oxo-6-phenyl-1,3-oxazinan-6-yl)propyl methanesulfonate (234 mg, 0.24 mmol) in CH2Cl2 (3 mL) was added NaH (82 mg, 3.4 mmol) at 0° C. The mixture was stirred at rt for 30 min. Then N-methylacetamide (204 mg, 2.8 mmol) was added the above mixture. The formed mixture was stirred at 80° C. for 5 h. After the reaction was over, the reaction was quenched with water and the mixture was extracted with EtOAc. The combined organic phase was concentrated to give the crude product, which was purified by preparative TLC to give N-(3-((R)-3-((S)-1-(4-bromophenyl)ethyl)-2-oxo-6-phenyl-1,3-oxazinan-6-yl)propyl)-N-methylacetamide (150 mg, 68%). LC-MS Method 2 tR=1.50 min, m/z=497, 495, 475, 473. 1H NMR (400 MHz, CDCl3): δ=1.41 (m, 1H), 1.48 (t, 3H), 1.73 (m, 1H), 1.83-1.95 (m, 2H), 2.01 (m, 3H), 2.1-2.3 (m, 3H), 2.71 (m, 1H), 2.81 (s, 3H), 3.1 (m, 1H), 3.2 (m, 1H), 5.5 (m, 1H), 6.72 (m, 2H), 7.10 (m, 2H), 7.20 (m, 2H), 7.37 (m, 3H).

後処理

  1. stirringThe formed mixture was stirred at 80° C. for 5 h
  2. customwas quenched with water
  3. extractionthe mixture was extracted with EtOAc
  4. concentrationThe combined organic phase was concentrated
  5. customto give the crude product, which
  6. customwas purified by preparative TLC

出典と根拠

ORDレコード
ord-d5dddd0661e64d4fa85478311af69631
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680093B2

反応ノート

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