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Methanol → HCID 86201264、化合物

HRID 2270557
ノート
印刷プレビュー

反応式

HRID 2270557 の反応式
C([O:3][C:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:6]=1[O:14][CH2:15][CH3:16])C.O1CCCC1.CO.[BH4-].[Li+]>O>[CH2:15]([O:14][C:6]1[C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=[CH:10][C:5]=1[CH2:4][OH:3])[CH3:16]
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 887MethanolHCID 8028TetrahydrofuranHCID 4148881Lithium borohydrideHCID 54007593HCID 54007593、化合物

生成物 1

HCID 86201264HCID 86201264、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of the compound (117 mg) obtained in Example 417a, tetrahydrofuran (5 ml) and methanol (2 ml), lithium borohydride (10.7 mg) was added. The reaction mixture was stirred at room temperature for 15 h, and, after addition of water, concentrated under reduced pressure. To the resulting residue, 2 N HCl was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:2) to give the titled compound quantitatively.

後処理

  1. additionwas added
  2. concentrationconcentrated under reduced pressure
  3. additionTo the resulting residue, 2 N HCl was added
  4. extractionthe mixture was subjected to extraction with ethyl acetate
  5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  6. dry with materialdried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:2)

出典と根拠

ORDレコード
ord-cf682594faad4d5d82d93ab8fc3530a7
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06331553B1

反応ノート

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