Methanol → 2,2'-((5-(1-(((4-(Trifluoromethyl)benzyl)oxy)imino)ethyl)oxazol-2-yl)azanediyl)diacetic acid

HRID 68321ノート

反応式

HRID 68321 の反応式
[F:1][C:2]([F:33])([F:32])[C:3]1[CH:31]=[CH:30][C:6]([CH2:7][O:8][N:9]=[C:10]([C:12]2[O:16][C:15]([N:17]([CH2:24][C:25]([O:27]CC)=[O:26])[CH2:18][C:19]([O:21]CC)=[O:20])=[N:14][CH:13]=2)[CH3:11])=[CH:5][CH:4]=1.CO.O.[OH-].[Li+]>C1COCC1>[F:33][C:2]([F:1])([F:32])[C:3]1[CH:4]=[CH:5][C:6]([CH2:7][O:8][N:9]=[C:10]([C:12]2[O:16][C:15]([N:17]([CH2:24][C:25]([OH:27])=[O:26])[CH2:18][C:19]([OH:21])=[O:20])=[N:14][CH:13]=2)[CH3:11])=[CH:30][CH:31]=1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 86699628Diethyl 2,2'-((5-(1-(((4-(trifluoromethyl)benzyl)oxy)imino)ethyl)oxazol-2-yl)azanediyl)diacetate

生成物 1

HCID 765282152,2'-((5-(1-(((4-(Trifluoromethyl)benzyl)oxy)imino)ethyl)oxazol-2-yl)azanediyl)diacetic acid収率 97.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the product of step 3 (295 mg, 0.62 mmoles) in a mixture of THF (6 ml), methanol (2 ml) and water (2 ml), lithium hydroxide (105 mg, 1.25 mmoles) was added and the reaction mixture was stirred at ambient temperature for 4 hours. The solvents were evaporated under reduced pressure. The residue was dissolved in water and acidified with 1N HCl. White solid seperated was filtered and washed with water & dried over P2O5 under vacuum to give 250 mg (82%) of title product as off white solid.

後処理

  1. additionwas added
  2. customThe solvents were evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. customWhite solid seperated
  5. filtrationwas filtered
  6. washwashed with water
  7. dry with materialdried over P2O5 under vacuum

出典と根拠

ORDレコード
ord-8117eb18b54444b9ae5ee61fff184666
出典データセット
uspto-grants-2014_09
特許番号
US08822414B2

反応ノート

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