2-Aminobenzyl alcohol → HCID 57474716、化合物

HRID 391680

反応式

HRID 391680 の反応式
[N+:1]([C:4]1[C:5]([C:28](OCC)=[O:29])=[N:6][C:7]([NH:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[CH2:26][OH:27])=[N:8][C:9]=1[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[O:17][CH3:18])([O-])=O.ClC1N=C([C:40](OCC)=[O:41])C([N+]([O-])=O)=C(NC2C=CC=CC=2OC)N=1.[NH2:57]C1C=CC=CC=1CO.C(N(C(C)C)CC)(C)C>CN(C)C=O>[OH:27][CH2:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[NH:19][C:7]1[N:8]=[C:9]2[C:4]([NH:1][C:40](=[O:41])[N:10]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])=[C:5]([C:28]([NH2:57])=[O:29])[N:6]=1

参加物

6

反応物 4

HCID 214392-Aminobenzyl alcoholHCID 81531DiisopropylethylamineHCID 57474573HCID 57474573、化合物HCID 57474717HCID 57474717、化合物

生成物 1

HCID 57474716HCID 57474716、化合物収率 86%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Ethyl 5-nitro-2-(2-(hydroxymethyl)phenylamino)-6-(2-methoxyphenylamino)pyrimidine-4-carboxylate. Ethyl 2-chloro-6-(2-methoxyphenylamino)-5-nitropyrimidine-4-carboxylate (See Example 30.A) (0.300 g, 0.852 mmol), 2-aminobenzyl alcohol (0.125 g, 1.2 mmol) and diisopropylethylamine (0.296 g) were reacted according to General Procedure C, except at room temperature and in dimethylformamide (5 ml). The crude reaction mixture was condensed and purified using Biotage chromatography (60 to 100% EtOAc in hexanes) to afford the title compound (0.323 g, 86%). MS (ESI) m/z 440.5 [M+1]+.

後処理

  1. customThe crude reaction mixture
  2. customcondensed
  3. custompurified

出典と根拠

ORDレコード
ord-0f74feac840e4890ab527f36cd025e46
出典データセット
uspto-grants-2013_02
特許番号
US08383634B2

関連ノート

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