Lithium Hydroxide → HCID 86658522、化合物

HRID 471372ノート

反応式

HRID 471372 の反応式
[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

参加物

6

反応物 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

生成物 1

HCID 86658522HCID 86658522、化合物収率 83%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-17d0c5b2df5a4afd82bcfb079c7a05ae
出典データセット
uspto-grants-2014_01
特許番号
US08633134B2

反応ノート

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