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Potassium thiocyanate → 3-Thiocyanato-2,2-dimethyl-1-propanesulfonamide

HRID 465933
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HRID 465933 반응식
S(O[CH2:12][C:13]([CH3:20])([CH3:19])[CH2:14][S:15]([NH2:18])(=[O:17])=[O:16])(C1C=CC(C)=CC=1)(=O)=O.[S-:21][C:22]#[N:23].[K+]>CN(C)C=O>[S:21]([CH2:12][C:13]([CH3:20])([CH3:19])[CH2:14][S:15]([NH2:18])(=[O:16])=[O:17])[C:22]#[N:23]
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참가 물질

4

반응물 2

HCID 516872Potassium thiocyanateHCID 100646893-Tosyloxy-2,2-dimethyl-1-propanesulfonamide

생성물 1

HCID 104430543-Thiocyanato-2,2-dimethyl-1-propanesulfonamide수율 21.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 6.2 g of 3-tosyloxy-2,2-dimethyl-1-propanesulfonamide and 3.75 g of potassium thiocyanate in 30 ml of dimethylformamide was stirred at 130°-140° C. for 6 hours, and then concentrated to dryness. A mixture of dichloromethane and methanol (9:1)was added to the residue, followed by filtration to remove insoluble material. The filtrate was concentrated and the residue was subjected to a column chromatography, eluting with chloroform-ethyl acetate (2:1). The relevant fractions were concentrated to obtain 0.87 g of 3-thiocyanato-2,2-dimethyl-1-propanesulfonamide as yellow oil.

후처리

  1. concentrationconcentrated to dryness
  2. additionA mixture of dichloromethane and methanol (9
  3. addition1)was added to the residue
  4. filtrationfollowed by filtration
  5. customto remove insoluble material
  6. concentrationThe filtrate was concentrated
  7. washeluting with chloroform-ethyl acetate (2:1)
  8. concentrationThe relevant fractions were concentrated

출처 및 근거

ORD 기록
ord-870789b9d8184a9ba1438d557e25e1f5
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05155108

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