Hydrochloric Acid → HCID 23359138, 화합물

HRID 232871노트

반응식

HRID 232871 반응식
[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]

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 23359208HCID 23359208, 화합물

생성물 1

HCID 23359138HCID 23359138, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-49401f63030540308abde24b1e69a386
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

반응 노트

불러오는 중…