Hydrochloric Acid → HCID 178477659、化合物

HRID 238583ノート

反応式

HRID 238583 の反応式
[OH-].[K+].C(S([C:8]1[CH:13]=[CH:12][C:11]([S:14]([CH2:17][CH3:18])(=[O:16])=[O:15])=[CH:10][N:9]=1)(=O)=O)C.[O:19]1CCCC1.Cl>O>[CH2:17]([S:14]([C:11]1[CH:12]=[CH:13][C:8]([OH:19])=[N:9][CH:10]=1)(=[O:16])=[O:15])[CH3:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14797Potassium HydroxideHCID 132780152,5-Bis(ethylsulfonyl)pyridine

生成物 1

HCID 178477659HCID 178477659、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A solution of potassium hydroxide (11.0 g, 196 mmol, 50%) in water was added to a suspension of 2,5-bis-ethanesulfonyl-pyridine (12.0 g, 45.6 mmol, prepared using the method described above) in water and tetrahydrofuran (100 mL, 1:1, v/v). After being heated at reflux for 1 hour, the mixture was acidified with 0.5 N hydrochloric acid to pH 3 and concentrated in vacuo to remove the solvent. The residue was triturated with boiling ethanol (150 mL) and filtered. The filtrates were concentrated in vacuo to afford the crude product which was used in the next step without further purification.

後処理

  1. customprepared
  2. temperatureAfter being heated
  3. temperatureat reflux for 1 hour
  4. concentrationconcentrated in vacuo
  5. customto remove the solvent
  6. customThe residue was triturated with boiling ethanol (150 mL)
  7. filtrationfiltered
  8. concentrationThe filtrates were concentrated in vacuo

出典と根拠

ORDレコード
ord-f2ecad1a18ee4e4e9b16ee032d053956
出典データセット
uspto-grants-2014_02
特許番号
US08642629B2

反応ノート

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