Ethanol → HCID 21401589、化合物

HRID 1730137ノート

反応式

HRID 1730137 の反応式
[O:1]1[CH2:22][CH:2]1[CH2:3][CH2:4][CH2:5][N:6]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19]CC)=[O:18])[S:7]([CH3:10])(=[O:9])=[O:8].[OH-:23].[Na+].[CH2:25](O)[CH3:26]>O>[OH:23][CH:2]([CH2:22][O:1][CH2:25][CH3:26])[CH2:3][CH2:4][CH2:5][N:6]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])[S:7]([CH3:10])(=[O:8])=[O:9]

参加物

5

反応物 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 21401575ethyl 7-[N-(4,5-epoxypentyl)methanesulfonamido]heptanoate

生成物 1

HCID 21401589HCID 21401589、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of ethyl 7-[N-(4,5-epoxypentyl)-methanesulfonamido]heptanoate (7.0 g., 0.02 mole) in ethanol (150 ml.) is added sodium hydroxide (1.84 g., 0.046 mole) dissolved in water (15 ml.). This solution is stirred at room temperature for 18 hours, then concentrated to one-half volume under reduced pressure. Water (150 ml.) is added and this aqueous solution is extracted with ether (2 × 100 ml.). The aqueous layer is then acidified (dilute hydrochloric acid) and extracted with ethyl acetate (2 × 150 ml.). The organic phase is washed with brine, dried over sodium sulfate, then evaporated in vacuo. The yield of subject compound is 4.0 g. (54%) of pale yellow oil.

後処理

  1. concentrationconcentrated to one-half volume under reduced pressure
  2. additionWater (150 ml.) is added
  3. extractionthis aqueous solution is extracted with ether (2 × 100 ml.)
  4. extractionextracted with ethyl acetate (2 × 150 ml.)
  5. washThe organic phase is washed with brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-4406cec655db48f99b6279a157f49d54
出典データセット
uspto-grants-1976_11
特許番号
US03991106

反応ノート

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