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

Hydrochloric Acid → 7-(Benzyloxy)-4-methyl-2H-chromene

HRID 217425
ノート
印刷プレビュー

反応式

HRID 217425 の反応式
[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13](=O)[CH2:14][CH2:15][O:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:20][Mg]Br.[NH4+].[Cl-].Cl>C1COCC1>[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([CH3:20])=[CH:14][CH2:15][O:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 45218987-(benzyloxy)-3,4-dihydro-2H-1-benzopyran-4-oneHCID 178418573HCID 178418573、化合物2 回

生成物 1

HCID 584387087-(Benzyloxy)-4-methyl-2H-chromene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

7-(benzyloxy)-2,3-dihydro-4H-chromen-4-one was dissolved in THF, a solution (0.97 M, 5 mL) of methylmagnesium bromide in THF was added dropwise thereto at 0° C., followed by stirring at room temperature for 1 hour, and a solution (0.97 M, 5 mL) of methylmagnesium bromide in THF was added dropwise thereto, followed by stirring at room temperature for 2 hours. To the reaction liquid was added a saturated aqueous NH4Cl solution and subsequently 2 M hydrochloric acid (20 mL), followed by stirring at room temperature for 2 hours and then extracting with EtOAc three times. The organic layer was combined, washed with water and brine, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=95:5 to 90:10) to obtain 7-(benzyloxy)-4-methyl 2H-chromene (445 mg) as a colorless transparent liquid.

後処理

  1. customat 0° C.
  2. stirringby stirring at room temperature for 2 hours
  3. customTo the reaction liquid
  4. stirringby stirring at room temperature for 2 hours
  5. extractionextracting with EtOAc three times
  6. washwashed with water and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=95:5 to 90:10)

出典と根拠

ORDレコード
ord-efe7b9a6971a47059481d8a847ed0fa9
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08193378B2

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