3-(Pyridin-3-yl)propanoic acid → HCID 45261551、化合物

HRID 128648

反応式

HRID 128648 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][C:7]3[CH:18]=[CH:17][CH:16]=[CH:15][C:8]=3[CH2:9][N:10]([C:11]([NH:13][NH2:14])=[O:12])[C:4]=2[CH:3]=1.[N:21]1[CH:26]=[CH:25][CH:24]=[C:23]([CH2:27][CH2:28][C:29](O)=[O:30])[CH:22]=1>C(O)(=O)C>[ClH:1].[O:30]=[C:29]([NH:14][NH:13][C:11]([N:10]1[CH2:9][C:8]2[CH:15]=[CH:16][CH:17]=[CH:18][C:7]=2[O:6][C:5]2[CH:19]=[CH:20][C:2]([Cl:1])=[CH:3][C:4]1=2)=[O:12])[CH2:28][CH2:27][C:23]1[CH:22]=[N:21][CH:26]=[CH:25][CH:24]=1

参加物

4

反応物 2

HCID 2596243-(Pyridin-3-yl)propanoic acidHCID 135604618-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, hydrazide

生成物 1

HCID 45261551HCID 45261551、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

The experiment described above in Example 7 was repeated on a five mmol scale with 8-chlorodibenz[b,f][1,41oxazepine-10(11H)-carboxylic acid, hydrazide (1), prepared as described above in Example 1, and 3-(3-pyridyl)propionic acid. The yield of the reaction product was 0.75 g (34%). The free base was dissolved in 5 mL of acetic acid (HOAc) and filtered. To the filtrate was added 5 mL of 6N HCl dioxane. The hydrochloride salt was precipitated from the reaction by the addition of Et2O. The resultant solid product was collected by filtration and dried in an Abderhalden drying pistol. Analysis calculated for C22H20N4O3Cl2 : C, 57.53; H, 4.39; N, 12.20; Cl, 15.44. Found: C, 57.35; H, 4.45; N, 12.08; Cl, 15.58.

後処理

  1. customprepared
  2. filtrationfiltered
  3. additionTo the filtrate was added 5 mL of 6N HCl dioxane
  4. customThe hydrochloride salt was precipitated from the reaction by the addition of Et2O
  5. filtrationThe resultant solid product was collected by filtration
  6. customdried in an Abderhalden
  7. customdrying pistol

出典と根拠

ORDレコード
ord-f085158a85954a30a31044d6807651fc
出典データセット
uspto-grants-1995_11
特許番号
US05464830

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