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Hydrochloric Acid → HCID 23320192、化合物

HRID 280856
ノート
印刷プレビュー

反応式

HRID 280856 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][N:9]2[CH2:14][CH2:13][N:12]([CH:15]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:11][CH2:10]2)[CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:35][S:36]([Cl:39])(=[O:38])=[O:37].[ClH:40]>C(Cl)(Cl)Cl>[ClH:39].[ClH:40].[CH3:35][S:36]([NH:1][C:2]1[N:7]=[C:6]([CH2:8][N:9]2[CH2:10][CH2:11][N:12]([CH:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:13][CH2:14]2)[CH:5]=[CH:4][CH:3]=1)(=[O:38])=[O:37]
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 4

HCID 313Hydrochloric AcidHCID 8471Triethylamine2 回HCID 31297Methanesulfonyl chloride2 回HCID 13362831HCID 13362831、化合物

生成物 1

HCID 23320192HCID 23320192、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 1-(6-aminopyridin-2-ylmethyl)-4-benzhydrylpiperazine (3.58 g) and triethylamine (1.01 g) in chloroform (20 ml) was dropwise added methanesulfonylchloride (1.15 g) at 5° to 10° C. under cooling with stirring, which was continued at the same temperature for 1 hour. To the resultant mixture, additional triethylamine (0.51 g) and methanesulfonyl chloride (0.57 g) were added successively. The mixture was stirred for 1.5 hours. The reaction mixture was washed with water, dried and evaporated in vacuo. The resulting oily product was subjected to column chromatography on silica gel eluting with a mixture of chloroform and methanol (30:1). The fractions containing the desired compound were combined and evaporated in vacuo to give a residue. According to a conventional manner, the residue was converted to hydrochloric acid salt, which was recrystallized from a mixture of methanol and diethyl ether to give 1-(6-methanesulfonylaminopyridin-2-ylmethyl)-4-benzhydrylpiperazine dihydrochloride (0.97 g). mp: 201°-202° C.

後処理

  1. customat 5° to 10° C.
  2. temperatureunder cooling
  3. stirringThe mixture was stirred for 1.5 hours
  4. washThe reaction mixture was washed with water
  5. customdried
  6. customevaporated in vacuo
  7. additionThe resulting oily product was subjected to column chromatography on silica gel eluting with a mixture of chloroform and methanol (30:1)
  8. additionThe fractions containing the desired compound
  9. customevaporated in vacuo
  10. customto give a residue
  11. customwas recrystallized from a mixture of methanol and diethyl ether

出典と根拠

ORDレコード
ord-806b4c3b9a6d4e78bed737039b1b785a
出典データセット
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04591590

反応ノート

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