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N-bromobutanimide → (4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one

HRID 1815633
ノート
印刷プレビュー

反応式

HRID 1815633 の反応式
[CH2:1]([Mg]Cl)[CH2:2][CH2:3][CH3:4].[CH2:7]([C@@H:14]1[CH2:18][O:17][C:16](=[O:19])[N:15]1[C:20](=[O:27])/[CH:21]=[CH:22]/[CH2:23][CH2:24][CH2:25][CH3:26])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Br:28]N1C(=O)CCC1=O>C1COCC1.CSC>[CH2:7]([C@@H:14]1[CH2:18][O:17][C:16](=[O:19])[N:15]1[C:20](=[O:27])[C@H:21]([Br:28])[CH:22]([CH2:1][CH2:2][CH2:3][CH3:4])[CH2:23][CH2:24][CH2:25][CH3:26])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 67184N-bromobutanimideHCID 66929717(4R)-4-benzyl-3-[(E)-2-heptenoyl]-1,3-oxazolidin-2-oneHCID 178418265HCID 178418265、化合物

生成物 1

HCID 66929892(4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one

試薬・触媒・溶媒 2

HCID 1068Dimethyl Sulfide溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
-15 °C

実験手順

A slurry of copper bromide(I) dimethyl sulfide complex (5.132 g, 24.967 mmol) in THF (60 mL) and dimethyl sulfide (30 mL) as a co-solvent was cooled to −40° C. and n-butyl magnesium chloride (25 mL, 49.93 mmol) was added dropwise for 10 min and stirred for 20 min while warming to −15° C. The black slurry was cooled to −40° C. and (4R)-4-benzyl-3-[(E)-2-heptenoyl]-1,3-oxazolidin-2-one (6 g, 20.80 mmol) was added dropwise over 10 min as a solution in THF (20 mL) at −40° C. The reaction was let warm up to 25° C. overnight (20 h). N-Bromosuccinimide (7.407 g, 41.61 mmol) was added portionwise to a cold −78° C. solution of the black slurry. It was allowed to warm to 0° C. and was stirred for an additional 3 h. The reaction was quenched with a 1:1 solution of saturated ammonium carbonate and 0.5 N potassium bisulfate. The black slurry became greenish to blue. A precipitate formed (light blue). It was filtered. The mother liquor was diluted with ethyl acetate (150 mL) and the organic was dried over MgSO4, filtered, concentrated to obtain (4R)-4-benzyl-3-[(2R)-2-bromo-3-butylheptanoyl]-1,3-oxazolidin-2-one as a crude semi-solid (green) (8.49 g, 96.15%). Mass Spectrum (−ESI): 423 (M−H)−.

後処理

  1. temperatureThe black slurry was cooled to −40° C.
  2. temperatureThe reaction was let warm up to 25° C. overnight (20 h)
  3. temperatureto warm to 0° C.
  4. stirringwas stirred for an additional 3 h
  5. customThe reaction was quenched with a 1:1 solution of saturated ammonium carbonate and 0.5 N potassium bisulfate
  6. customA precipitate formed (light blue)
  7. filtrationIt was filtered
  8. additionThe mother liquor was diluted with ethyl acetate (150 mL)
  9. dry with materialthe organic was dried over MgSO4
  10. filtrationfiltered
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-c1f4bb7b4b124d8887a7dc58bffdc48f
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06878742B2

反応ノート

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