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

HRID 1358128노트

반응식

HRID 1358128 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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)−.

후처리

  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

출처 및 근거

ORD 기록
ord-7818474b8dfd4f4fba9485b5a435cc58
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06593480B2

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