Acetic Acid → HCID 178426257, 화합물

HRID 1470225노트

반응식

HRID 1470225 반응식
[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[N-:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1.[K+].C(O)(=O)C>O.C1COCC1>[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[NH:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 176Acetic Acid3회HCID 443866Pemirolast potassium

생성물 1

HCID 178426257HCID 178426257, 화합물수율 55.4%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

The free acid was prepared from pemirolast potassium (15.8 g; Chemtronica AB) by dissolution in a mixture of water (100 mL) and THF (80 mL) at room temperature and acidification with acetic acid (1 eq.; 17.5 g; 20% aq.). Firstly, ca. 1 mL of acetic acid was added and the obtained thin slurry was equilibrated for about 30 minutes. Thereafter the rest of the acetic acid was added slowly. The resultant thick slurry was diluted with water (50 mL) and equilibrated for 2 hours and then filtered and washed with water. The resultant solid was dried at 40° C. and under reduced pressure for 5-10 hours to yield 7.5 g of sub-title compound.

후처리

  1. waitequilibrated for 2 hours
  2. filtrationfiltered
  3. washwashed with water
  4. customThe resultant solid was dried at 40° C. and under reduced pressure for 5-10 hours

출처 및 근거

ORD 기록
ord-f921b390e5bf453ead57fc367ec01415
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006431B2

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