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Sodium Hydroxide → Butanoic acid, 4-((5-(1,2-dithiolan-3-yl)-1-oxopentyl)amino)-

HRID 849575
ノート
印刷プレビュー

反応式

HRID 849575 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][C:16]([O:18]C)=[O:17])=[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][C:16]([OH:18])=[O:17])=[O:11])[S:2]1
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 14798Sodium HydroxideHCID 18358048HCID 18358048、化合物

生成物 1

HCID 43043Butanoic acid, 4-((5-(1,2-dithiolan-3-yl)-1-oxopentyl)amino)-収率 45.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The reaction was effected as described in Example 49, but using 0.65 g of methyl 4-[5-(1,2-dithiolan-3yl)pentanoylamino]butanoate (prepared as described in Example 73), 13 ml of methanol and a 1N aqueous solution of sodium hydroxide. The solvent was removed from the reaction mixture by distillation under reduced pressure. Water was added to the residue. After neutralisation with 2N aqeous hydrochloric acid, the resulting mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. Ethyl acetate was removed from the extract by distillation under reduced pressure. The residue was recrystallized from ethyl acetate, to give 0.28 g of the title compound as yellow crystals, melting at 56 to 58° C.

後処理

  1. customThe solvent was removed from the reaction mixture by distillation under reduced pressure
  2. additionWater was added to the residue
  3. extractionAfter neutralisation with 2N aqeous hydrochloric acid, the resulting mixture was extracted with ethyl acetate
  4. washThe extract was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. customEthyl acetate was removed from the
  7. extractionextract by distillation under reduced pressure
  8. customThe residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-648e1b98bd0f4806844b046f565b9dda
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06013663

反応ノート

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