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Butyl isocyanate → HCID 13489816、化合物

HRID 1980776
ノート
印刷プレビュー

反応式

HRID 1980776 の反応式
[O:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:12]([NH2:15])(=[O:14])=[O:13])=[CH:4][CH:3]=[N:2]1.[CH2:16]([N:20]=[C:21]=[O:22])[CH2:17][CH2:18][CH3:19].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:16]([NH:20][C:21]([NH:15][S:12]([C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:5]1[O:1][N:2]=[CH:3][CH:4]=1)(=[O:13])=[O:14])=[O:22])[CH2:17][CH2:18][CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8110Butyl isocyanateHCID 11430Potassium CarbonateHCID 134898132-(Isoxazol-5-yl)benzenesulfonamide

生成物 1

HCID 13489816HCID 13489816、化合物収率 79.7%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A solution of 8.7 g of 2-(isoxazol-5-yl)benzenesulfonamide prepared in Example 5, 4.7 g of n-butyl isocyanate and 5.4 g of potassium carbonate in 125 ml of 2-butanone was refluxed for 7 hours. The resulting suspension was concentrated to dryness in vacuo. The residue was taken up in 200 ml of water and extracted once with 100 ml of ethyl ether. The aqueous layer was acidified with 2N HCl and the resulting suspension was extracted with methylene chloride. After drying the methylene chloride extract over sodium sulfate, the solvent was evaporated off under reduced pressure. The solid residue was recrystallized from acetonitrile to give 10 g of the title compound; m.p. 110°-113° C.

後処理

  1. concentrationThe resulting suspension was concentrated to dryness in vacuo
  2. extractionextracted once with 100 ml of ethyl ether
  3. extractionthe resulting suspension was extracted with methylene chloride
  4. dry with materialAfter drying the methylene chloride
  5. extractionextract over sodium sulfate
  6. customthe solvent was evaporated off under reduced pressure
  7. customThe solid residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-b0a98ca01eb4415b9698165eb243df13
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04511392

反応ノート

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