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Trifluoroacetic acid → N-(5-amino-2-methylphenyl)-4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamide

HRID 1465030
ノート
印刷プレビュー

反応式

HRID 1465030 の反応式
[CH:1]1([NH:4][C:5]2[C:6]3[S:13][CH:12]=[C:11]([C:14]([NH:16][C:17]4[CH:18]=[C:19]([NH:24]C(=O)OC(C)(C)C)[CH:20]=[CH:21][C:22]=4[CH3:23])=[O:15])[C:7]=3[N:8]=[CH:9][N:10]=2)[CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:24][C:19]1[CH:20]=[CH:21][C:22]([CH3:23])=[C:17]([NH:16][C:14]([C:11]2[C:7]3[N:8]=[CH:9][N:10]=[C:5]([NH:4][CH:1]4[CH2:2][CH2:3]4)[C:6]=3[S:13][CH:12]=2)=[O:15])[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67361287t-Butyl 3-(4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamido)-4-methylphenylcarbamate

生成物 1

HCID 67360673N-(5-amino-2-methylphenyl)-4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

t-Butyl 3-(4-(cyclopropylamino)thieno[3,2-d]pyrimidine-7-carboxamido)-4-methylphenylcarbamate (7 g, 15.93 mmol) was dissolved in DCM (80 mL), TFA (12 mL, 159.3 mmol) was added thereto, and the mixture was stirred at room temperature for 8 hours. After the reaction was completed, the reaction mixture was concentrated under reduced pressure to remove the organic solvent and the remaining TFA, and water (20 mL) was added thereto. The reaction mixture was neutralized with 2.0 N NaOH solution, and the resulting yellow solid was filtered and dried to obtain the title compound without further purification.

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customto remove the organic solvent
  3. additionthe remaining TFA, and water (20 mL) was added
  4. filtrationthe resulting yellow solid was filtered
  5. customdried

出典と根拠

ORDレコード
ord-e0c046fd91ce4bc289aba9f8c6b97a85
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999973B2

反応ノート

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