Acetic Acid → HCID 54343451、化合物

HRID 1381626ノート

反応式

HRID 1381626 の反応式
[CH3:1][C:2]1[C:3]([CH3:23])=[CH:4][C:5]2[O:9][C:8]([CH:10]=[CH:11][C:12]3[CH:21]=[CH:20][C:15]([C:16]([O:18]C)=[O:17])=[CH:14][CH:13]=3)=[N:7][C:6]=2[CH:22]=1.C(O)(=O)C.S(=O)(=O)(O)O>O>[CH3:1][C:2]1[C:3]([CH3:23])=[CH:4][C:5]2[O:9][C:8]([CH:10]=[CH:11][C:12]3[CH:21]=[CH:20][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=3)=[N:7][C:6]=2[CH:22]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 102316Benzoic acid, 4-[2-(5,6-dimethyl-2-benzoxazolyl)ethenyl]-, methyl ester

生成物 1

HCID 54343451HCID 54343451、化合物収率 89.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 3.0 g methyl 4-[(5,6-dimethyl-2-benzoxazolyl)vinyl]benzoate, 25 mL of acetic acid, 9.0 mL of concentrated sulfuric acid, and 7 mL of water is stirred and refluxed for three hours. The mixture is cooled and added to water. The product is collected by filtration, washed with water and air dried. The crude product is recrystallized from N,N-dimethylformamide to give 2.57 g of 4-[2-(5,6-dimethyl-2-benzoxazolyl)vinyl]benzoic acid, which melts at >300° C.

後処理

  1. temperaturerefluxed for three hours
  2. temperatureThe mixture is cooled
  3. filtrationThe product is collected by filtration
  4. washwashed with water and air
  5. customdried
  6. customThe crude product is recrystallized from N,N-dimethylformamide

出典と根拠

ORDレコード
ord-9ce406e63caa46fe8fd5db9efff1d59a
出典データセット
uspto-grants-1989_02
特許番号
US04803241

反応ノート

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