Hydrochloric Acid → HCID 53759290、化合物

HRID 1683050ノート

反応式

HRID 1683050 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=2)([C:14]#[N:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClS(N=[C:29]=[O:30])(=O)=O.Cl.[OH-:32].[Na+]>ClCCl>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11]2([N:16]([C:17]3[CH:18]=[CH:19][C:20]([F:23])=[CH:21][CH:22]=3)[C:29](=[O:30])[NH:15][C:14]2=[O:32])[CH2:12][CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 70918Chlorosulfonyl isocyanateHCID 30172221-Benzyl-4-((4-fluorophenyl)amino)piperidine-4-carbonitrile

生成物 1

HCID 53759290HCID 53759290、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Combine 1-benzyl-4-(4-fluoro-phenylamino)-piperidine-4-carbonitrile (32 mmol) and dichloromethane (100 mL). Add chlorosulfonyl isocyanate (20 mmol) in dropwise fashion with water bath cooling so as to maintain the temperature of the reaction mixture between 20° and 30° C. After 30 minutes, concentrate the reaction mixture in vacuo to obtain a residue. Add 1N HCl (100 mL) and heat at reflux for 1 h. Cool in an ice bath and adjust the pH to 5.5 using 5N NaOH. Filter to obtain a residue. Wash with diethyl ether and dry in vacuo. Purify to obtain the title compound.

後処理

  1. temperatureto maintain the temperature of the reaction mixture between 20° and 30° C
  2. concentrationconcentrate the reaction mixture in vacuo
  3. customto obtain a residue
  4. temperatureheat
  5. temperatureat reflux for 1 h
  6. temperatureCool in an ice bath
  7. filtrationFilter
  8. customto obtain a residue
  9. washWash with diethyl ether
  10. customdry in vacuo
  11. customPurify

出典と根拠

ORDレコード
ord-338e9e40099c4d65af55b4c63fe06f8b
出典データセット
uspto-grants-1997_06
特許番号
US05635510

反応ノート

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