Diisopropylethylamine → 3-(2-methoxy-pyrimidin-5-yl)-2-{[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidine-1-carbonyl]-amino}-propionic acid methyl ester

HRID 1177743ノート

反応式

HRID 1177743 の反応式
[CH3:1][O:2][C:3](=[O:15])[CH:4]([NH2:14])[CH2:5][C:6]1[CH:7]=[N:8][C:9]([O:12][CH3:13])=[N:10][CH:11]=1.C(N(C(C)C)CC)(C)C.C1C(=O)N(OC(ON2C(=O)CCC2=O)=O)[C:27](=[O:28])C1.[NH:43]1[CH2:48][CH2:47][CH:46]([N:49]2[CH2:58][C:57]3[C:52](=[CH:53][CH:54]=[CH:55][CH:56]=3)[NH:51][C:50]2=[O:59])[CH2:45][CH2:44]1>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:15])[CH:4]([NH:14][C:27]([N:43]1[CH2:44][CH2:45][CH:46]([N:49]2[CH2:58][C:57]3[C:52](=[CH:53][CH:54]=[CH:55][CH:56]=3)[NH:51][C:50]2=[O:59])[CH2:47][CH2:48]1)=[O:28])[CH2:5][C:6]1[CH:7]=[N:8][C:9]([O:12][CH3:13])=[N:10][CH:11]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 676246Di(succinimido) carbonateHCID 110425973-(Piperidin-4-yl)-3,4-dihydroquinazolin-2(1H)-oneHCID 59639681Methyl 2-amino-3-(2-methoxypyrimidin-5-yl)propanoate

生成物 1

HCID 588642893-(2-methoxy-pyrimidin-5-yl)-2-{[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidine-1-carbonyl]-amino}-propionic acid methyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-Amino-3-(2-methoxy-pyrimidin-5-yl)-propionic acid methyl ester (125 mg) and diisopropylethylamine (0.3 mL) in methylene chloride (2 mL, 0° C.) was added N,N′-disuccinimidyl carbonate (155 mg). After 30 min, 3-piperidin-4-yl-3,4-dihydro-1H-quinazolin-2-one (120 mg) in methylene chloride (2 mL) was added via canula. The reaction was warmed to room temperature and stirred overnight. The reaction was concentrated and purified by prep HPLC to give 99 mg (36%). Mass spec.: 469.10 (MH)+.

後処理

  1. concentrationThe reaction was concentrated
  2. custompurified by prep HPLC
  3. customto give 99 mg (36%)

出典と根拠

ORDレコード
ord-8be0cacde8ef4567a11631e32a7cbe4d
出典データセット
uspto-grants-2010_11
特許番号
US07842808B2

反応ノート

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