Methyl 4-(4-carbamoyl-2-ethoxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate → 4-(4-Carbamoyl-2-ethoxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylic acid

HRID 450530ノート

反応式

HRID 450530 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]2[C:12]3[C:19]([CH3:20])=[C:18]([C:21]([O:23]C)=[O:22])[S:17][C:13]=3[N:14]=[CH:15][N:16]=2)=[C:6]([O:25][CH2:26][CH3:27])[CH:5]=1)(=[O:3])[NH2:2]>[OH-].[NH4+]>[C:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]2[C:12]3[C:19]([CH3:20])=[C:18]([C:21]([OH:23])=[O:22])[S:17][C:13]=3[N:14]=[CH:15][N:16]=2)=[C:6]([O:25][CH2:26][CH3:27])[CH:5]=1)(=[O:3])[NH2:2]

参加物

3

反応物 1

HCID 46182171Methyl 4-(4-carbamoyl-2-ethoxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate

生成物 1

HCID 461820414-(4-Carbamoyl-2-ethoxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylic acid収率 31.3%

試薬・触媒・溶媒 1

HCID 14923Ammonium Hydroxide溶媒

反応条件

温度
150 °C

実験手順

A suspension of methyl 4-(4-carbamoyl-2-ethoxyphenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate (0.025 g, 0.06 mmol) in ammonium hydroxide (1.5 mL) was heated at 150° C. in a sealed-tube for 16 hours. The ammonium hydroxide was concentrated in vacuo and the residue redissolved in dimethyl sulfoxide. The sample was purified by reverse phase preparative HPLC to yield white solid (0.007 g, 29%).

後処理

  1. concentrationThe ammonium hydroxide was concentrated in vacuo
  2. dissolutionthe residue redissolved in dimethyl sulfoxide
  3. customThe sample was purified by reverse phase preparative HPLC

出典と根拠

ORDレコード
ord-12782c7a06fd494f8beeceb9be3933ed
出典データセット
uspto-grants-2013_07
特許番号
US08486953B2

反応ノート

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