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Methanol → (R)-(-)-2-(1-Isobutoxyethoxy)-1-propanol

HRID 2085627
ノート
印刷プレビュー

反応式

HRID 2085627 の反応式
[BH4-].[Na+].[CH2:3]([O:7][CH:8]([O:10][C@H:11]([CH3:19])[C:12](OCC(C)C)=[O:13])[CH3:9])[CH:4]([CH3:6])[CH3:5].CO.O>C1(C)C=CC=CC=1>[CH2:3]([O:7][CH:8]([O:10][C@H:11]([CH3:19])[CH2:12][OH:13])[CH3:9])[CH:4]([CH3:6])[CH3:5]
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 962WaterHCID 4311764Sodium borohydrideHCID 12994193Isobutyl (R)-(+)-2-(1-Isobutoxyethoxy)propionate

生成物 1

HCID 12994194(R)-(-)-2-(1-Isobutoxyethoxy)-1-propanol収率 85.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.0 g (0.024 mole) of sodium borohydride was suspended at room temperature in a solution of 5.0 g (0.02 mole) of isobutyl (R)-(+)-2-(1-isobutoxyethoxy)propionate dissolved in 20 ml of toluene. Thereto was dropwise added slowly 7.0 ml (0.12 mole) of methanol with stirring, so that the internal temperature of the reaction system could be kept at 40° C. After the completion of the dropwise addition, the resulting mixture was stirred at 40° C. for 7 hours, at room temperature overnight and at 60° C. for 2 hours to give rise to a reaction. To the reaction mixture was added 20 ml of water, followed by stirring for 0.5 hour. The organic layer was separated. The water layer was subjected to extraction with 20 ml of toluene. The two organic layers were combined and washed with 20 ml of water and 20 ml of a saturated aqueous sodium chloride solution in this order. The washed solution was dried over anhydrous sodium sulfate and then subjected to vacuum distillation to remove the solvent, whereby was obtained 3.0 g (yield: 84.4%) of an oily title compound (diastereomixture).

後処理

  1. customcould be kept at 40° C
  2. additionAfter the completion of the dropwise addition
  3. stirringthe resulting mixture was stirred at 40° C. for 7 hours, at room temperature overnight and at 60° C. for 2 hours
  4. customto give rise
  5. customto a reaction
  6. stirringby stirring for 0.5 hour
  7. customThe organic layer was separated
  8. extractionThe water layer was subjected to extraction with 20 ml of toluene
  9. washwashed with 20 ml of water and 20 ml of a saturated aqueous sodium chloride solution in this order
  10. dry with materialThe washed solution was dried over anhydrous sodium sulfate
  11. distillationsubjected to vacuum distillation
  12. customto remove the solvent

出典と根拠

ORDレコード
ord-6433e6bc2ef1491e84ba646899e79778
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06720463B1

反応ノート

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