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Sodium borohydride → HCID 53710797、化合物

HRID 1456683
ノート
印刷プレビュー

反応式

HRID 1456683 の反応式
[BH4-].[Na+].[O:3]=[C:4]1[C:17]2[CH:16]=[C:15]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:14]=[CH:13][C:12]=2[O:11][C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2>C(O)C>[OH:3][CH:4]1[C:17]2[CH:16]=[C:15]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:14]=[CH:13][C:12]=2[O:11][C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 12274127ethyl 9-oxo-9H-xanthene-2-acetate

生成物 1

HCID 53710797HCID 53710797、化合物収率 43%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

5.67 g (150 mmol) of sodium borohydride are added in portions to a solution of 14.2 g (50 mmol) of ethyl 9-oxo-9H-xanthene-2-acetate (Example 10d) in 130 ml of ethanol. The suspension is stirred at room temperature for 15 hours, subsequently diluted with 80 ml of ethanol and poured onto water. The product is extracted with ethyl acetate. The organic phases are washed with an aqueous saturated sodium chloride solution, combined, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. The solid residue is suspended in ethanol, the suspension is filtered and the product is dried under a high vacuum. 6.1 g (43%) of ethyl 9-hydroxy-9H-xanthene-2-acetate, melting point 214°-219° C., results as a white powder.

後処理

  1. additionpoured onto water
  2. extractionThe product is extracted with ethyl acetate
  3. washThe organic phases are washed with an aqueous saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated on a vacuum rotary evaporator
  6. filtrationthe suspension is filtered
  7. customthe product is dried under a high vacuum

出典と根拠

ORDレコード
ord-5543cc3645bd491cbdaed7cbae0f0b1e
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05844024

反応ノート

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