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Hydrochloric Acid → N-[2-(3-cyano-1-propen-1-yl)phenylsulfonyl]N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea

HRID 1030014
ノート
印刷プレビュー

反応式

HRID 1030014 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([N:10](C2C=CC=CC=2)[C:11](=[O:13])[O-])[N:4]=1.[C:20]([CH2:22][CH:23]=[CH:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[S:31]([NH2:34])(=[O:33])=[O:32])#[N:21].N12CCCCC1C=NCCC2.Cl>O1CCOCC1.O>[C:20]([CH2:22][CH:23]=[CH:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[S:31]([NH:34][C:11]([NH:10][C:5]1[N:4]=[C:3]([O:2][CH3:1])[N:8]=[C:7]([CH3:9])[N:6]=1)=[O:13])(=[O:33])=[O:32])#[N:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 199952694-Methoxy-6-methyl-1,3,5-triazin-2-ylphenylcarbamateHCID 540327212-(3-Cyano-1-propen-1-yl)phenylsulfonamide

生成物 1

HCID 53795420N-[2-(3-cyano-1-propen-1-yl)phenylsulfonyl]N'-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)urea収率 66.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

5.2 g of N-(4methoxy-6-methyl-1,3,5-triazin-2yl)phenylcarbamate are added to a solution of 4.45 g of 2-(3-cyano-1propen-1-yl)phenylsulfonamide and 3.3 ml of 1,5-diazabicyclo[5,4,0]undec-5-ene in 80 ml of dioxan, and the mixture is stirred for 15 hours at 20°-25° C. The reaction mixture is then taken up in 350 ml of water and the aqueous solution is acidified to pH 2 with 2N HCl and extracted with ethyl acetate. The organic extracts are combined and concentrated. The oily orange-coloured residue is dissolved in a very small amount of acetone. About 20 ml of diethyl ether are added to this solution, which is diluted dropwise with haxane until the onset of crystallisation. The mixture is subsequently further cooled and the precipitated crystals are isolated by filtration. Yield: 5.2 g of the title compound with a melting point of 142°-143° C.

後処理

  1. extractionextracted with ethyl acetate
  2. concentrationconcentrated
  3. dissolutionThe oily orange-coloured residue is dissolved in a very small amount of acetone
  4. additionAbout 20 ml of diethyl ether are added to this solution, which
  5. additionis diluted dropwise with haxane until the onset of crystallisation
  6. temperatureThe mixture is subsequently further cooled
  7. customthe precipitated crystals are isolated by filtration

出典と根拠

ORDレコード
ord-59b552e843a0472cb3494538ac9f5415
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05104440

反応ノート

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