Lithium Hydroxide → HCID 86658522, 화합물

HRID 471372노트

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HRID 471372 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:27]([F:30])([F:29])[F:28])[O:13][N:12]=[C:11]([C:14]3[CH:25]=[CH:24][C:17]([C:18]([N:21]([CH3:23])[CH3:22])=[N:19][OH:20])=[C:16]([CH3:26])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Li+].[OH-].S(OC)(O[CH3:37])(=O)=O>CN(C=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:27]([F:28])([F:30])[F:29])[O:13][N:12]=[C:11]([C:14]3[CH:25]=[CH:24][C:17]([C:18]([N:21]([CH3:22])[CH3:23])=[N:19][O:20][CH3:37])=[C:16]([CH3:26])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

6

반응물 3

HCID 3939Lithium HydroxideHCID 6497Dimethyl SulfateHCID 1363411624-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-N'-hydroxy-2,N,N-trimethyl-benzamidine

생성물 1

HCID 86658522HCID 86658522, 화합물수율 83%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-[5-(3,5-Dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]-N′-hydroxy-2,N,N-trimethyl-benzamidine (200 mg) in DMF (5 mL) was added a solution of LiOH (31 mg) in water (2 mL), before adding dimethyl sulfate (0.21 mL, 0.27 g). The mixture was stirred at room temperature over night and poured onto water. The aqueous layer was extracted with MTBE and the combined organic layers were washed with water, dried (Na2SO4) and evaporated to yield the title compound (170 mg, 83%).

후처리

  1. additionpoured onto water
  2. extractionThe aqueous layer was extracted with MTBE
  3. washthe combined organic layers were washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-17d0c5b2df5a4afd82bcfb079c7a05ae
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633134B2

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