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Sodium Methoxide → 1-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1, 2,4-triazol-1-yl)-2-butylsulfonyl]-4-(4-methyl-4H-1,2,4-triazol-3-ylmethyl) piperazine

HRID 274607
ノート
印刷プレビュー

反応式

HRID 274607 の反応式
Cl.Cl.[F:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[C@@:11]([OH:29])([CH2:23][N:24]1[CH:28]=[N:27][CH:26]=[N:25]1)[C@H:12]([S:14]([N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1)(=[O:16])=[O:15])[CH3:13].Cl.Cl[CH2:32][C:33]1[N:37]([CH3:38])[CH:36]=[N:35][N:34]=1.C[O-].[Na+]>CO>[F:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[C@@:11]([OH:29])([CH2:23][N:24]1[CH:28]=[N:27][CH:26]=[N:25]1)[C@H:12]([S:14]([N:17]1[CH2:22][CH2:21][N:20]([CH2:32][C:33]2[N:37]([CH3:38])[CH:36]=[N:35][N:34]=2)[CH2:19][CH2:18]1)(=[O:16])=[O:15])[CH3:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10942334Sodium MethoxideHCID 186592571-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)-2-butylsulfonyl]piperazine.dihydrochloride2 回HCID 223819093-(chloromethyl)-4-methyl-4H-1,2,4-triazole hydrochloride

生成物 1

HCID 542808911-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1, 2,4-triazol-1-yl)-2-butylsulfonyl]-4-(4-methyl-4H-1,2,4-triazol-3-ylmethyl) piperazine収率 25.8%

試薬・触媒・溶媒

1
HCID 887Methanol溶媒2 回

反応条件

温度
70 °C

実験手順

In methanol (6 ml) were dissolved 1-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)-2-butylsulfonyl]piperazine-dihydrochloride (Compound 20, 0.40 g) and 3-chloromethyl-4-methyl-4H1,2,4-triazole.hydrochloride (255 mg). To the solution was added 1N-methanol solution of sodium methylate (3.69 ml), and the mixture was heated at 70° C. for 14 hours, then the reaction mixture was concentrated. The concentrate was dissolved in dichloromethane (30 ml), washed with water, dried and concentrated. The concentrate was recrystallized from ethyl acetate to give 1-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1, 2,4-triazol-1-yl)-2-butylsulfonyl]-4-(4-methyl-4H-1,2,4-triazol-3-ylmethyl) piperazine (Compound 26, 108 mg) as pale yellow crystals.

後処理

  1. concentrationthe reaction mixture was concentrated
  2. dissolutionThe concentrate was dissolved in dichloromethane (30 ml)
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe concentrate was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-a59c09cb34ee419c8919fb697eaf4bb6
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05389663

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート