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

Anisole → HCID 58155274、化合物

HRID 1929493
ノート
印刷プレビュー

反応式

HRID 1929493 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C@@:8]2([CH3:26])[N:13](CC3C=CC(OC)=CC=3)[C:12](=[O:23])[C:11]([CH3:25])([CH3:24])[O:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.C1(OC)C=CC=CC=1.FC(F)(F)S(O)(=O)=O.C(=O)([O-])O.[Na+]>FC(F)(F)C(O)=O>[Br:1][C:2]1[CH:3]=[C:4]([C@@:8]2([CH3:26])[NH:13][C:12](=[O:23])[C:11]([CH3:25])([CH3:24])[O:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=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 4

HCID 7519AnisoleHCID 62406Trifluoromethanesulfonic acidHCID 516892Sodium BicarbonateHCID 58155245HCID 58155245、化合物

生成物 1

HCID 58155274HCID 58155274、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
73 °C

実験手順

A solution of (R)-5-(3-bromo-phenyl)-4-(4-methoxy-benzyl)-2,2,5-trimethyl-morpholin-3-one (487 mg, 1.2 mmol) and anisole (2.305 g, 21.3 mmol) in trifluoroacetic acid (6 ml) was treated dropwise with trifluoromethanesulfonic acid (1.19 ml). After complete addition, the violet reaction mixture was heated at 73° C. for 23 hours. The cooled reaction mixture was poured into a saturated solution of sodium hydrogen-carbonate which was extracted with ethyl acetate. The organic layer was separated, washed with brine, dried over sodium sulfate, and evaporated at reduced pressure. The crude product was purified by chromatography on silica gel using a gradient of heptane and ethyl acetate=100/0 to 66/34 as the eluent. The product containing fractions (550 mg, orange foam) were collected and engaged in the next step without further purification and characterization.

後処理

  1. additionAfter complete addition
  2. customThe cooled reaction mixture
  3. extractionwas extracted with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated at reduced pressure
  8. customThe crude product was purified by chromatography on silica gel using a gradient of heptane and ethyl acetate=100/0 to 66/34 as the eluent
  9. additionThe product containing fractions (550 mg, orange foam)
  10. customwere collected
  11. customengaged in the next step without further purification and characterization

出典と根拠

ORDレコード
ord-f6d0572062204153ab894cd56e1f092f
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08188079B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート