HCID 86641478、化合物 → {5-Chloro-1-[(5-chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[4,3-d]pyrimidin-3-yl}-acetic acid

HRID 472739ノート

反応式

HRID 472739 の反応式
C([O:5][C:6](=[O:36])[CH2:7][N:8]1[C:13](=[O:14])[C:12]2[C:15]([Cl:19])=[N:16][CH:17]=[CH:18][C:11]=2[N:10]([CH2:20][C:21](=[O:34])[NH:22][C:23]2[CH:28]=[C:27]([Cl:29])[C:26]([O:30][CH3:31])=[CH:25][C:24]=2[O:32][CH3:33])[C:9]1=[O:35])(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[Cl:19][C:15]1[C:12]2[C:13](=[O:14])[N:8]([CH2:7][C:6]([OH:36])=[O:5])[C:9](=[O:35])[N:10]([CH2:20][C:21](=[O:34])[NH:22][C:23]3[CH:28]=[C:27]([Cl:29])[C:26]([O:30][CH3:31])=[CH:25][C:24]=3[O:32][CH3:33])[C:11]=2[CH:18]=[CH:17][N:16]=1

参加物

4

反応物 1

HCID 86641478HCID 86641478、化合物2 回

生成物 1

HCID 59317708{5-Chloro-1-[(5-chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[4,3-d]pyrimidin-3-yl}-acetic acid

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 6422Trifluoroacetic acid溶媒

実験手順

To a vial containing a solution of {5-Chloro-1-[(5-chloro-2,4-dimethoxy-phenylcarbamoyl)-methyl]-2,4-dioxo-1,4-dihydro-2H-pyrido[4,3-d]pyrimidin-3-yl}-acetic acid tert-butyl ester (Intermediate T) (10.1 mg, 0.019 mmol) in DCM (1 ml), TFA (1 ml) is added. The reaction mixture is stirred at RT for 2 hours, transferred to a 10 ml round bottomed flask, diluted with a minimal amount of DCM and concentrated in vacuo. The residue is taken up in 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 compound.

後処理

  1. additionis added
  2. customtransferred to a 10 ml round bottomed flask
  3. concentrationconcentrated in vacuo
  4. concentrationconcentrated in vacuo
  5. concentrationonce with MeOH, the solvent being concentrated in vacuo each time

出典と根拠

ORDレコード
ord-f4fcef4606b445939faef957f9cb1d05
出典データセット
uspto-grants-2014_01
特許番号
US08633211B2

反応ノート

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