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 450530노트

반응식

HRID 450530 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 14923Ammonium Hydroxide용매

반응 조건

온도
150 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-12782c7a06fd494f8beeceb9be3933ed
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486953B2

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