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

Water → (5,6,7,8-Tetrahydroquinoxalin-2-yl)methanol

HRID 385523
ノート
印刷プレビュー

反応式

HRID 385523 の反応式
[N:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[N:4]=[CH:3][C:2]=1[C:11](OCC)=[O:12].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.O>O1CCCC1>[N:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[N:4]=[CH:3][C:2]=1[CH2:11][OH:12]
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 962WaterHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydride2 回HCID 57815216Ethyl 5,6,7,8-tetrahydroquinoxaline-2-carboxylate

生成物 1

HCID 57815285(5,6,7,8-Tetrahydroquinoxalin-2-yl)methanol収率 78.5%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of 0.16 g of ethyl 5,6,7,8-tetrahydroquinoxaline-2-carboxylate in 1.5 mL of tetrahydrofuran, 29 mg of lithium aluminum hydride was added under cooling with ice, the mixture was stirred for 45 minutes, 29 mg of lithium aluminum hydride was further added thereto, and the mixture was stirred for 30 minutes. Thereto were added ethyl acetate and water, the insoluble substance was filtered off, sodium chloride was added to a filtrate, the organic layer was separated, and the aqueous layer was extracted with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 0.10 g of (5,6,7,8-tetrahydroquinoxalin-2-yl)methanol as a brown solid.

後処理

  1. temperatureunder cooling with ice
  2. stirringthe mixture was stirred for 30 minutes
  3. filtrationthe insoluble substance was filtered off
  4. additionsodium chloride was added to a filtrate
  5. customthe organic layer was separated
  6. extractionthe aqueous layer was extracted with ethyl acetate
  7. washthe resultant solution was washed with a saturated aqueous sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-9ee83d6333d9471bbe420832069d8bbc
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367831B2

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