Hydrochloric Acid → HCID 23359138、化合物

HRID 232871ノート

反応式

HRID 232871 の反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].C([C:10]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[C:12]([CH2:19][O:20][C:21]2[CH:26]=CC(O)=[CH:23][CH:22]=2)[CH:11]=1)#N.O.Cl.[N:30]1C=CC=C[CH:31]=1>>[C:5]([O:4][C:1]1[CH:23]=[CH:22][C:21]([O:20][CH2:19][C:12]2([C:31]#[N:30])[CH:11]=[CH:10][CH:18]=[CH:17][CH:13]2[C:14]([OH:16])=[O:15])=[CH:26][CH:2]=1)(=[O:7])[CH3:6]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 23359208HCID 23359208、化合物

生成物 1

HCID 23359138HCID 23359138、化合物

実験手順

Under ice cooling and stirring, 5.5 ml of acetic anhydride was added to 5.2 g of 4-cyano-2-(4-hydroxyphenoxy)methylbenzoic acid obtained in Reference example 23 dissolved in 15.6 ml of pyridine and the mixture was stirred at the same temperature for 1.5 hours. Water was added to the reaction mixture and the mixture was adjusted to about pH 2 with conc. hydrochloric acid and extracted with ethyl acetate. Then, the organic layer was washed with a saturated saline solution, 1N-hydrochloric acid and further a saturated saline solution and then dried over anhydrous sodium sulfate. The solvent was removed to obtain 5.36 g of a crude product of the title compound.

後処理

  1. customobtained in Reference example 23
  2. stirringthe mixture was stirred at the same temperature for 1.5 hours
  3. extractionextracted with ethyl acetate
  4. washThen, the organic layer was washed with a saturated saline solution, 1N-hydrochloric acid
  5. dry with materialfurther a saturated saline solution and then dried over anhydrous sodium sulfate
  6. customThe solvent was removed

出典と根拠

ORDレコード
ord-49401f63030540308abde24b1e69a386
出典データセット
uspto-grants-1997_01
特許番号
US05591752

反応ノート

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