Water → HCID 67503155、化合物

HRID 1887199ノート

反応式

HRID 1887199 の反応式
[C:1]([O:5][C:6](=[O:20])[C@@H:7]([NH:10][C:11]([C:13]1[C:18]([NH2:19])=[CH:17][CH:16]=[CH:15][N:14]=1)=[O:12])[CH2:8][CH3:9])([CH3:4])([CH3:3])[CH3:2].[C:21](N1C=CN=C1)(N1C=CN=C1)=[O:22].N12CCCN=C1CCCCC2.O>O1CCCC1>[C:1]([O:5][C:6](=[O:20])[C@@H:7]([N:10]1[C:11](=[O:12])[C:13]2[N:14]=[CH:15][CH:16]=[CH:17][C:18]=2[NH:19][C:21]1=[O:22])[CH2:8][CH3:9])([CH3:2])([CH3:3])[CH3:4]

参加物

6

反応物 4

HCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 67502797HCID 67502797、化合物

生成物 1

HCID 67503155HCID 67503155、化合物収率 55%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 217 mg of (S)-2-[(3-amino-pyridine-2-carbonyl)-amino]-butyric acid tert-butyl ester in tetrahydrofuran (10 mL) is treated with 259 mg of 1,1′-carbonyldiimidazole and 0.018 mL of 1,8-diazabicyclo[5.4.0]undec-7-ene. The mixture is stirred at room temperature for 16 h. Then the reaction mixture is added water (1 mL) and the resulting mixture is concentrated and purified by flash chromatography on silica gel to give 130 mg (55%) of (S)-2-(2,4-dioxo-1,4-dihydro-2H-pyrido[3,2-d]pyrimidin-3-yl)-butyric acid tert-butyl ester.

後処理

  1. concentrationthe resulting mixture is concentrated
  2. custompurified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-e2c1fd4d254b4278b2b97c065f81029a
出典データセット
uspto-grants-2013_08
特許番号
US08501749B2

反応ノート

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