5-Amino-3-methylisoxazole → HCID 135980549、化合物

HRID 1910670ノート

反応式

HRID 1910670 の反応式
[C:1]([C:3]([C:23](=O)[CH3:24])=[CH:4][C:5]1[O:13][C:12]2[CH:11]=[CH:10][N:9]=[C:8]([NH:14][C:15](=[O:22])[C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:7]=2[CH:6]=1)#[N:2].[CH3:26][C:27]1[CH:31]=[C:30]([NH2:32])[O:29][N:28]=1>CC(O)C>[C:1]([C:3]1[CH:4]([C:5]2[O:13][C:12]3[CH:11]=[CH:10][N:9]=[C:8]([NH:14][C:15](=[O:22])[C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)[C:7]=3[CH:6]=2)[C:31]2[C:27]([CH3:26])=[N:28][O:29][C:30]=2[NH:32][C:23]=1[CH3:24])#[N:2]

参加物

4

反応物 2

HCID 845905-Amino-3-methylisoxazoleHCID 67154537N-{2-(2-Cyano-3-oxobut-1-en-1-yl)furo[3,2-c]pyridin-4-yl}benzamide

生成物 1

HCID 135980549HCID 135980549、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 200 mg (0.604 mmol) N-{2-(2-cyano-3-oxobut-1-en-1-yl)furo[3,2-c]pyridin-4-yl}benzamide (Example 4A), 59 mg (0.604 mmol) 3-methyl-1,2-oxazol-5-amine and a trace amount of powdered 4 Å molecular sieve in 2-propanol (2 ml) was stirred at 90° C. for 12 h. Upon cooling, the mixture was concentrated under reduced pressure, and the residue was directly purified by preparative RP-HPLC (methanol/water+0.1% TFA gradient, final mixture 100% methanol) to yield 64 mg (26% of th.) of the racemic title compound.

後処理

  1. temperatureUpon cooling
  2. concentrationthe mixture was concentrated under reduced pressure
  3. customthe residue was directly purified by preparative RP-HPLC (methanol/water+0.1% TFA gradient, final mixture 100% methanol)

出典と根拠

ORDレコード
ord-d45579c2915140dd8fc3a89e986c5f89
出典データセット
uspto-grants-2013_12
特許番号
US08604028B2

反応ノート

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