Hydrochloric Acid → 2-Methyl-1,3-benzoxazole-4-carboxylic acid

HRID 560310

反応式

HRID 560310 の反応式
[OH-].[K+].C([O:5][C:6]([C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[O:16][C:15]([CH3:17])=[N:14][C:13]=12)=[O:7])C.Cl>CO>[CH3:17][C:15]1[O:16][C:12]2[C:13](=[C:8]([C:6]([OH:7])=[O:5])[CH:9]=[CH:10][CH:11]=2)[N:14]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 593168402-Methyl-benzooxazole-4-carboxylic acid ethyl ester

生成物 1

HCID 183546282-Methyl-1,3-benzoxazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

At 0° C. an aq. KOH solution (1.0 M, 2.40 mL) is added to a solution of 2-methyl-benzoxazole-4-carboxylic acid ethyl ester (0.98 mmol) in MeOH (5.0 mL) and stirred for 30 min. The mixture is allowed to reach RT, stirred for additional 60 min and made acidic by addition of aq. HCl (2.0 M). After removal of MeOH under reduced pressure the obtained precipitate is filtered off to give the desired product which is dried in vacuo. 1H-NMR (DMSO-d6): δ=2.64 (s, 3H); 7.41 (t, J=8.0 Hz, 1H); 7.83 (d, J=7.8 Hz, 1H); 7.88 (d, J=8.0 Hz, 1H); 12.8 (bs, 1H).

後処理

  1. customto reach RT
  2. stirringstirred for additional 60 min
  3. customAfter removal of MeOH under reduced pressure the obtained precipitate
  4. filtrationis filtered off

出典と根拠

ORDレコード
ord-3ac663708b3540fc9dc064623712b8d0
出典データセット
uspto-grants-2011_11
特許番号
US08063099B2

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