Hydrochloric Acid → HCID 178463287、化合物

HRID 1912466ノート

反応式

HRID 1912466 の反応式
Cl.O1CCOCC1.CN(C)S([N:13]1[CH:17]=[CH:16][C:15]([C:18]([C:27]2[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=2)([NH:20]S(C(C)(C)C)=O)[CH3:19])=[N:14]1)(=O)=O>CO>[Cl:33][C:29]1[CH:28]=[C:27]([C:18]([NH2:20])([C:15]2[CH:16]=[CH:17][NH:13][N:14]=2)[CH3:19])[CH:32]=[CH:31][CH:30]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 668253223-[1-(3-Chloro-phenyl)-1-(2-methyl-propane-2-sulfinylamino)-ethyl]-pyrazole-1-sulfonic acid dimethylamide

生成物 1

HCID 178463287HCID 178463287、化合物収率 86%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

Hydrochloric acid 4 M in dioxane (19.79 mL, 79.15 mmol) was added to a solution of 3-[1-(3-chloro-phenyl)-1-(2-methyl-propane-2-sulfinylamino)-ethyl]-pyrazole-1-sulfonic acid dimethylamide (2.29 g, 5.28 mmol) in MeOH (5 mL) and the mixture was stirred at 80° C. in a sealed tube for 18 hours. The solvent was evaporated in vacuo. The residue was poured into NaHCO3 (aq. sat. solution) and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo to yield rac-1-(3-chloro-phenyl)-1-(1H-pyrazol-3-yl)-ethylamine (1 g, 86% yield) as a pale yellow solid which was used in the next step without further purification.

後処理

  1. customThe solvent was evaporated in vacuo
  2. additionThe residue was poured into NaHCO3 (aq. sat. solution)
  3. extractionextracted with DCM
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvents evaporated in vacuo

出典と根拠

ORDレコード
ord-89c34f2e4f5040b4a33d7a44b5bcb358
出典データセット
uspto-grants-2013_12
特許番号
US08609660B2

反応ノート

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