Hydrochloric Acid → HCID 90046213、化合物

HRID 1482910ノート

反応式

HRID 1482910 の反応式
[F:1][C:2]([F:21])([F:20])[O:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[N:14]=[C:13]([C:15]([O:17]CC)=[O:16])[CH:12]=[N:11]2)=[CH:6][CH:5]=1.[Li+].[OH-].O.Cl>C1COCC1.CO>[F:21][C:2]([F:1])([F:20])[O:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[N:14]=[C:13]([C:15]([OH:17])=[O:16])[CH:12]=[N:11]2)=[CH:8][CH:9]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 90046196HCID 90046196、化合物

生成物 1

HCID 90046213HCID 90046213、化合物収率 81.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 2-(4-(trifluoromethoxy)phenyl)-2H-1,2,3-triazole-4-carboxylate (127 mg, 422 μmol, Eq: 1.00) in THF (5 ml) and MeOH (1.00 ml) was added LiOH 1M (843 μl, 843 μmol, Eq: 2). The mixture was stirred overnight. To the residue was added water and 1 N HCl (pH:1), this aqueous phase was extracted two times with ethyl acetate, the resulting organic layers were combined and washed with brine, then dried over MgSO4, filtered and concentrated to give the desired compound (94 mg, 81.6%) as a white solid.

後処理

  1. extractionthis aqueous phase was extracted two times with ethyl acetate
  2. washwashed with brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6a6546c0844b46e693257fca7095d14a
出典データセット
uspto-grants-2016_08
特許番号
US09416127B2

反応ノート

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