Sodium Carbonate → 2,2-Diethoxythioacetamide

HRID 1860392노트

반응식

HRID 1860392 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 27947342,2-Diethoxythioacetamide수율 66.1%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-037d3a3fce9b483eb552b0c43bec90a2
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06531466B2

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