Sodium Carbonate → 2,2-Diethoxythioacetamide

HRID 1860392ノート

反応式

HRID 1860392 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]>C1COCC1.CC(=O)OCC>[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 3

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

生成物 1

HCID 27947342,2-Diethoxythioacetamide収率 66.1%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a suspension of phosphorus pentasulfide (27 g) in dry THF (100 ml) at 0° C. under vigorous stirring, Na2CO3 (13 g) was added. The reaction mixture was stirred for 30 min at 0° C. and for 30 min at r.t., then diethoxyacetamide (6 g) was added and stirring was continued at r.t. for 70 h. The reaction was then diluted with EA, washed with 10% Na3PO4, brine, dried over Na2SO4 and the solvent removed in vacuo. The crude residue was purified by flash-chromatography (EE/PE 1/1) to give the title compound as a white solid (4.4 g).

後処理

  1. additionwas added
  2. stirringstirring
  3. waitwas continued at r.t. for 70 h
  4. washwashed with 10% Na3PO4, brine
  5. dry with materialdried over Na2SO4
  6. customthe solvent removed in vacuo
  7. customThe crude residue was purified by flash-chromatography (EE/PE 1/1)

出典と根拠

ORDレコード
ord-037d3a3fce9b483eb552b0c43bec90a2
出典データセット
uspto-grants-2003_03
特許番号
US06531466B2

反応ノート

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