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Hydrochloric Acid → HCID 10513496、化合物

HRID 2210434
ノート
印刷プレビュー

反応式

HRID 2210434 の反応式
[CH:1]([NH:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][C:6]=1[S:11]([NH2:14])(=[O:13])=[O:12])([CH3:3])[CH3:2].[CH2:15]=O.Cl>C(O)(C)C.C(OCC)(=O)C>[CH:1]([N:4]1[C:5]2[CH:10]=[CH:9][N:8]=[CH:7][C:6]=2[S:11](=[O:13])(=[O:12])[NH:14][CH2:15]1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10632459HCID 10632459、化合物

生成物 1

HCID 10513496HCID 10513496、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate触媒HCID 3776Isopropanol溶媒

実験手順

A mixture of 1 g of 4-isopropylaminopyridine-3- sulfonamide (Preparation 3) and 1 g of paraformaldehyde in 20 cm3 of isopropanol to which 10 drops of ethyl acetate saturated with gaseous HCl have been added is brought to reflux for 3 hours. After cooling, the crystalline precipitate is filtered and washed with isopropanol. The precipitate is dissolved in 150 cm3 of hot methanol. The possible insoluble material is filtered. The filtrate is concentrated to dryness and the residue is taken up in 30 cm3 of water. The aqueous suspension is adjusted to a pH of 7-7.5 (NaHCO3) and the precipitate corresponding to the title compound is filtered, washed with water and dried.

後処理

  1. additionhave been added
  2. temperatureto reflux for 3 hours
  3. temperatureAfter cooling
  4. filtrationthe crystalline precipitate is filtered
  5. washwashed with isopropanol
  6. dissolutionThe precipitate is dissolved in 150 cm3 of hot methanol
  7. filtrationThe possible insoluble material is filtered
  8. concentrationThe filtrate is concentrated to dryness
  9. filtrationthe precipitate corresponding to the title compound is filtered
  10. washwashed with water
  11. customdried

出典と根拠

ORDレコード
ord-7a8afa0d1438446ba6d7884e93c5a6d7
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05459138

反応ノート

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