Ethyl Acetate → 2,2-Diethoxythioacetamide

HRID 1860385

反応式

HRID 1860385 の反応式
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:2].C(=O)([O-])[O-].[Na+].[Na+].[CH2:21]([O:23][CH:24]([O:28][CH2:29][CH3:30])[C:25]([NH2:27])=O)[CH3:22].CC(=O)OCC>C1COCC1>[CH2:21]([O:23][CH:24]([O:28][CH2:29][CH3:30])[C:25]([NH2:27])=[S:2])[CH3:22]

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 14817Phosphorus sulfide (P2S5)HCID 1007652,2-Diethoxyacetamide

生成物 1

HCID 27947342,2-Diethoxythioacetamide収率 90.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred mixture of P2S5 (45 g) in THF (300 ml) at 23°, sodium carbonate (21.5 g) was added. At the mixture, vigorously stirred, 2,2-diethoxyacetamide (10 g) was added. After 24 h a 10% aqueous solution of Na3PO4 (200 ml), EA (300 ml) and CH (300 ml) were respectively added. The aqueous layer was washed with EA and united to the organic layer. This was washed with water until clarification, dried and the solvent evaporated under reduce pressure. The crude residue was purified by flash chromatography (eluting with CH-EA 1:1) to give the title compound as a white solid (10 g).

後処理

  1. additionwere respectively added
  2. washThe aqueous layer was washed with EA
  3. washThis was washed with water until clarification
  4. customdried
  5. customthe solvent evaporated
  6. customThe crude residue was purified by flash chromatography (eluting with CH-EA 1:1)

出典と根拠

ORDレコード
ord-fa9db38bfdff4928a25e16fdd5ca99f6
出典データセット
uspto-grants-2003_03
特許番号
US06531466B2

関連ノート

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