ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrogen Bromide → Methyl 2-bromo-3-[3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]propionate

HRID 1584344
ノート
印刷プレビュー

反応式

HRID 1584344 の反応式
N([O-])=O.[Na+].[F:5][C:6]1[CH:7]=[C:8]([CH:10]=[CH:11][C:12]=1[O:13][CH2:14][C:15]1[N:16]=[C:17]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[O:18][C:19]=1[CH3:20])N.[BrH:27].[C:28]([O:32][CH3:33])(=[O:31])[CH:29]=[CH2:30]>O.[Cu]=O.CO.CC(C)=O>[Br:27][CH:29]([CH2:30][C:8]1[CH:10]=[CH:11][C:12]([O:13][CH2:14][C:15]2[N:16]=[C:17]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[O:18][C:19]=2[CH3:20])=[C:6]([F:5])[CH:7]=1)[C:28]([O:32][CH3:33])=[O:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 260Hydrogen BromideHCID 7294Methyl AcrylateHCID 108594853-Fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 10983188Methyl 2-bromo-3-[3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]propionate収率 76.8%

試薬・触媒・溶媒 4

HCID 14829
Copper oxide
触媒
HCID 180Acetone溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒

実験手順

A solution of sodium nitrite (NaNO2) (3.1 g) in water (5 ml) was added dropwise, at temperature ranging from 0 to 5° C., to a mixture of 3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)aniline (12.3 g), aqueous HBr (47%, 28.4 g) and acetone (150 ml)-methanol (50 ml). The mixture was stirred for 25 minutes at the same temperature range, to which was added methyl acrylate (21.3 g). The mixture was heated at temperatures ranging from 30 to 35° C., to which was then added copper oxide (Cu2O) (0.05 g) at the same temperature range. The whole mixture was vigorously stirred. The reaction mixture was stirred for further 30 minutes, which was then concentrated under reduced pressure. To the concentrate was added aqueous ammonia, which was subjected to extraction with ethyl acetate. The ethyl acetate layer was washed with water, which was then dried (MgSO4), followed by distilling off the solvent under reduced pressure. The residue was subjected to column chromatography on silica gel. From the fraction eluted with ethyl acetate-hexane (1:4), was obtained methyl 2-bromo-3-[3-fluoro-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)phenyl]propionate (14.2 g) as an oily product.

後処理

  1. temperatureThe mixture was heated at temperatures
  2. customranging from 30 to 35° C., to which
  3. stirringThe whole mixture was vigorously stirred
  4. stirringThe reaction mixture was stirred for further 30 minutes
  5. concentrationwhich was then concentrated under reduced pressure
  6. additionTo the concentrate was added aqueous ammonia, which
  7. extractionwas subjected to extraction with ethyl acetate
  8. washThe ethyl acetate layer was washed with water, which
  9. dry with materialwas then dried (MgSO4)
  10. distillationby distilling off the solvent under reduced pressure
  11. washFrom the fraction eluted with ethyl acetate-hexane (1:4)

出典と根拠

ORDレコード
ord-9675195a8748402f8263bc6655c24c40
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05932601

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート