Cumylamine → HCID 57737267, 화합물

HRID 549433노트

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HRID 549433 반응식
[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14](O)=[O:15])=[CH:13][C:9]=2[C:8]([NH:17][C:18](=[O:33])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[NH:25][C:26]([C:28]2[NH:29][CH:30]=[CH:31][CH:32]=2)=[O:27])=[N:7]1)=[O:5])[CH3:2].F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.CCN(C(C)C)C(C)C.[C:65]([NH2:74])([C:68]1[CH:73]=[CH:72][CH:71]=[CH:70][CH:69]=1)([CH3:67])[CH3:66]>CN(C=O)C.CCOC(C)=O>[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14](=[O:15])[NH:74][C:65]([CH3:67])([C:68]3[CH:73]=[CH:72][CH:71]=[CH:70][CH:69]=3)[CH3:66])=[CH:13][C:9]=2[C:8]([NH:17][C:18](=[O:33])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[NH:25][C:26]([C:28]2[NH:29][CH:30]=[CH:31][CH:32]=2)=[O:27])=[N:7]1)=[O:5])[CH3:2]

참가 물질

7

반응물 4

HCID 68509CumylamineHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 57737264HCID 57737264, 화합물

생성물 1

HCID 57737267HCID 57737267, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 3-{2-[(1H-Pyrrole-2-carbonyl)-amino]-benzoylamino}-thieno[2,3-c]pyrazole-1,5-dicarboxylic acid 1-ethyl ester (198.5 mg, 0.4246 mmol), 2-(1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (TBTU, 204 mg, 0.6369 mmol), DIEA (0.29 mL, 1.6984 mmol) and cumylamine (115 mg, 0.8492 mmol) in DMF (10 mL) was stirred at room temperature. After 2 hours the mixture was diluted with AcOEt (40 mL) and washed with saturated NaHCO3, water and brine. The organic layer was dried over Na2SO4 and evaporated to give 495 mg of crude that was used in the next step without further purification, LC-MS: Rt 7.36; [M+H]+ 585.

후처리

  1. washwashed with saturated NaHCO3, water and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customevaporated
  4. customto give 495 mg of crude that
  5. customwas used in the next step without further purification, LC-MS

출처 및 근거

ORD 기록
ord-0cca8dc2289842eea1b6bd14e2ea49e5
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943654B2

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