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{1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[3,4-d]pyrimidin-3-yl}-acetic acid tert-butyl ester → {1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[3,4-d]pyrimidin-3-yl}-acetic acid

HRID 472740
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인쇄 미리보기

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HRID 472740 반응식
C([O:5][C:6](=[O:35])[CH2:7][N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][N:17]=[CH:18][C:11]=2[N:10]([CH2:19][C:20](=[O:33])[NH:21][C:22]2[CH:27]=[C:26]([Cl:28])[C:25]([O:29][CH3:30])=[CH:24][C:23]=2[O:31][CH3:32])[C:9]1=[O:34])(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[Cl:28][C:26]1[C:25]([O:29][CH3:30])=[CH:24][C:23]([O:31][CH3:32])=[C:22]([NH:21][C:20]([CH2:19][N:10]2[C:11]3[CH:18]=[N:17][CH:16]=[CH:15][C:12]=3[C:13](=[O:14])[N:8]([CH2:7][C:6]([OH:35])=[O:5])[C:9]2=[O:34])=[O:33])[CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 68591872{1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[3,4-d]pyrimidin-3-yl}-acetic acid tert-butyl ester2회

생성물 1

HCID 59317715{1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[3,4-d]pyrimidin-3-yl}-acetic acid

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 6422Trifluoroacetic acid용매

실험 절차

To a vial containing a solution of {1-[(5-Chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[3,4-d]pyrimidin-3-yl}-acetic acid tert-butyl ester (Intermediate V) (15 mg, 0.029 mmol) in DCM (1 ml), TFA (1 ml) is added. The mixture is stirred at RT overnight. The reaction mixture is then transferred to a 10 ml round bottomed flask, diluted with a minimal amount of DCM and concentrated in vacuo. This process is repeated once with DCM, twice with EtOAc, and once with MeOH, the solvent being concentrated in vacuo each time, finally giving the title, [M+H]+ 448.93.

후처리

  1. additionis added
  2. customThe reaction mixture is then transferred to a 10 ml round bottomed flask
  3. concentrationconcentrated in vacuo
  4. concentrationonce with MeOH, the solvent being concentrated in vacuo each time
  5. customfinally giving the title, [M+H]+ 448.93

출처 및 근거

ORD 기록
ord-df3b5711aed44185807392589d886346
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08633211B2

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