Methanesulfonyl chloride → Methyl 5-methanesulfonylamino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

HRID 2269800ノート

反応式

HRID 2269800 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:12]2[C:17]([O:18][CH2:19][O:20][CH3:21])=[CH:16][CH:15]=[CH:14][C:13]=2[O:22][CH3:23])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].[CH3:24][S:25](Cl)(=[O:27])=[O:26]>N1C=CC=CC=1>[CH3:24][S:25]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:12]2[C:17]([O:18][CH2:19][O:20][CH3:21])=[CH:16][CH:15]=[CH:14][C:13]=2[O:22][CH3:23])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8])(=[O:27])=[O:26]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 18188782Methyl 5-amino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

生成物 1

HCID 18189252Methyl 5-methanesulfonylamino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of Example 32B (10 g, 34.8 mmol), in pyridine (50 mL) at room temperature was treated with methanesulfonyl chloride (2.7 mL, 34.8 mmol), stirred at room temperature for 16 hours, and concentrated. The concentrate was treated with ethyl acetate (100 mL), and the resulting solution was washed with 2N HCl, dried (Na2SO4), filtered, and concentrated. The concentrate was recrystallized from ethanol to provide the desired product. MS (ESI(−)Q1MS) m/z 394 (M−H)−.

後処理

  1. concentrationconcentrated
  2. additionThe concentrate was treated with ethyl acetate (100 mL)
  3. washthe resulting solution was washed with 2N HCl
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was recrystallized from ethanol

出典と根拠

ORDレコード
ord-297a8da4f83d47e68200283e16c6310b
出典データセット
uspto-grants-2001_12
特許番号
US06329534B1

反応ノート

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