Diisopropylethylamine → HCID 178502528、化合物

HRID 1056535ノート

反応式

HRID 1056535 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[C:10]([C:11]2[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=2[O:18][CH3:19])=[CH:9][C:8](=[O:20])[NH:7][C:6]1=[S:21].[NH2:22][C:23](=[N:29][C:30](=[O:33])[O:31][CH3:32])N1C=CC=N1.C(N(CC)C(C)C)(C)C>CN(C=O)C>[CH3:32][O:31][C:30](=[O:33])[N:29]=[C:23]([NH2:22])[NH:1][CH2:2][CH2:3][CH2:4][N:5]1[C:10]([C:11]2[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=2[O:18][CH3:19])=[CH:9][C:8](=[O:20])[NH:7][C:6]1=[S:21]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 72641374methyl [amino(1H-pyrazol-1-yl)methylidene]carbamateHCID 866847011-(3-aminopropyl)-6-(5-chloro-2-methoxyphenyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one

生成物 1

HCID 178502528HCID 178502528、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-(3-aminopropyl)-6-(5-chloro-2-methoxyphenyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (prepared in an analogous manner to Example 6; 50 mg, 0.14 mmol) and methyl [amino(1H-pyrazol-1-yl)methylidene]carbamate (28 mg, 0.16 mmol) in DMF (0.46 mL) was added N,N-diisopropylethylamine (0.024 mL, 0.14 mmol) at room temperature, and the mixture was stirred for 72 hours. The solvent was removed under reduced pressure, the residue was dissolved in DMSO (0.9 mL) and purified using mass-triggered automatic purification to give the title compound (4.9 mg) MS (ES+) 425.9 [M+H]+. Retention time: 1.54 min; Method: XBridge C18 5 um 4.6×50 mm, 95% H2O/5% MeCN linear to 5% H2O/95% MeCN over 4.0 min, HOLD at 5% H2O/95% MeCN to 5.0 min. (0.03% NH4OH). Flow rate: 2 mL/min.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in DMSO (0.9 mL)
  3. custompurified
  4. customautomatic purification

出典と根拠

ORDレコード
ord-357d80843e594c79b28337cd7745f988
出典データセット
uspto-grants-2016_07
特許番号
US09399626B2

反応ノート

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