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

HRID 465933
ノート
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反応式

HRID 465933 の反応式
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]
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 516872Potassium thiocyanateHCID 100646893-Tosyloxy-2,2-dimethyl-1-propanesulfonamide

生成物 1

HCID 104430543-Thiocyanato-2,2-dimethyl-1-propanesulfonamide収率 21.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-870789b9d8184a9ba1438d557e25e1f5
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05155108

反応ノート

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