Diisopropylethylamine → HCID 178502528, 화합물

HRID 1056535노트

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HRID 1056535 반응식
[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]

참가 물질

5

반응물 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

생성물 1

HCID 178502528HCID 178502528, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-357d80843e594c79b28337cd7745f988
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09399626B2

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