Sodium Hydroxide → 5-{[5-(1,2-Dithiolan-3-yl)pentanoyl]amino}pentanoic acid

HRID 849590ノート

反応式

HRID 849590 の反応式
[S:1]1[CH2:5][CH2:4][CH:3]([CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19]C)=[O:18])=[O:11])[S:2]1.[OH-].[Na+]>CO>[S:1]1[CH2:5][CH2:4][CH:3]([CH2:6][CH2:7][CH2:8][CH2:9][C:10]([NH:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])=[O:11])[S:2]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18357981HCID 18357981、化合物

生成物 1

HCID 183580775-{[5-(1,2-Dithiolan-3-yl)pentanoyl]amino}pentanoic acid収率 53.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The reaction was carried out as described in Example 49, but using 0.65 g of methyl 5-[5-(1,2-dithiolan-3-yl)pentanoylamino]pentanoate (prepared as described in Example 118), 13 ml of methanol and 5.09 ml of a 1 N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by evaporation under reduced pressure, and water was added to the residue. The mixture was neutralized by the addition of 2 N aqueous hydrochloric acid, after which it was extracted with ethyl acetate. The extraction solution was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. The ethyl acetate was removed from the extraction solution by evaporation under reduced pressure, and the residue was recrystallized from ethyl acetate, to obtain 0.33 g of the title compound as pale yellowish green crystals, melting at 98 to 100° C.

後処理

  1. customThe solvent was removed from the reaction mixture by evaporation under reduced pressure, and water
  2. additionwas added to the residue
  3. additionThe mixture was neutralized by the addition of 2 N aqueous hydrochloric acid
  4. extractionafter which it was extracted with ethyl acetate
  5. washThe extraction solution was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe ethyl acetate was removed from the extraction solution by evaporation under reduced pressure
  8. customthe residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-8d2393d226ea439e9541123c5f01307b
出典データセット
uspto-grants-2000_01
特許番号
US06013663

反応ノート

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