Acetic Acid → HCID 178426257、化合物

HRID 1470225ノート

反応式

HRID 1470225 の反応式
[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

参加物

5

反応物 2

HCID 176Acetic Acid3 回HCID 443866Pemirolast potassium

生成物 1

HCID 178426257HCID 178426257、化合物収率 55.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f921b390e5bf453ead57fc367ec01415
出典データセット
uspto-grants-2015_04
特許番号
US09006431B2

反応ノート

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