Sodium Hydroxide → tert-butyl 2-(2-(N-cyclopropyl-4-methoxy-2,6-dimethylphenylsulfonamido)ethoxy)acetate

HRID 2059885노트

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HRID 2059885 반응식
[OH-].[Na+].[CH:3]1([N:6]([CH2:20][CH2:21][OH:22])[S:7]([C:10]2[C:15]([CH3:16])=[CH:14][C:13]([O:17][CH3:18])=[CH:12][C:11]=2[CH3:19])(=[O:9])=[O:8])[CH2:5][CH2:4]1.[C:23]([O:27][C:28](=[O:31])[CH2:29]Br)([CH3:26])([CH3:25])[CH3:24]>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH:3]1([N:6]([CH2:20][CH2:21][O:22][CH2:29][C:28]([O:27][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:31])[S:7]([C:10]2[C:15]([CH3:16])=[CH:14][C:13]([O:17][CH3:18])=[CH:12][C:11]=2[CH3:19])(=[O:9])=[O:8])[CH2:4][CH2:5]1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 79177tert-Butyl bromoacetateHCID 43577600N-Cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide

생성물 1

HCID 59820154tert-butyl 2-(2-(N-cyclopropyl-4-methoxy-2,6-dimethylphenylsulfonamido)ethoxy)acetate수율 90%

시약·촉매·용매 2

HCID 70681Tetrabutylammonium Chloride촉매HCID 1140Toluene용매

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온도
25 °C

실험 절차

tetra-n-Butylammonium chloride (0.33 eq) and 35% sodium hydroxide solution (18 ml) were added to a solution of N-cyclopropyl-N-(2-hydroxyethyl)-4-methoxy-2,6-dimethylphenylsulfonamide (3.3 mmol) in toluene (18 ml), cooled to 0° C. tert-Butylbromoacetate (1.5 eq) was added slowly to this mixture at 0° C. On completion of the addition the mixture was stirred for 90 min at 25° C. until the reaction was complete. The organic phase was separated off, washed with water until a neutral pH was measured, dried over MgSO4, filtered and concentrated completely to obtain the desired product. Yield: 90%

후처리

  1. additionwas added slowly to this mixture at 0° C
  2. additionOn completion of the addition the mixture
  3. customThe organic phase was separated off
  4. washwashed with water until a neutral pH
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated completely

출처 및 근거

ORD 기록
ord-d47908948486495395945d089a19b03d
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08278319B2

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