Ammonia → HCID 59596671, 화합물

HRID 2264816노트

반응식

HRID 2264816 반응식
CC(OC([NH:8][C@@H:9]([CH2:14][C:15]#[C:16][C:17]1[CH:22]=[CH:21][C:20]([NH:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[F:31])=[CH:19][CH:18]=1)[C:10]([O:12][CH3:13])=[O:11])=O)(C)C.N>C(Cl)Cl.O>[NH2:8][C@@H:9]([CH2:14][C:15]#[C:16][C:17]1[CH:22]=[CH:21][C:20]([NH:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[F:31])=[CH:19][CH:18]=1)[C:10]([O:12][CH3:13])=[O:11]

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 59596674HCID 59596674, 화합물

생성물 1

HCID 59596671HCID 59596671, 화합물수율 89.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A solution of methyl (2S)-2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)-5-(4-{[(2-fluorophenyl)methyl]amino}phenyl)-4-pentynoate (D65, 192 mg, 0.450 mmol) in DCM containing 5% TFA (10.5 ml) was stirred at room temperature for 4.5 h. Then 28% NH3 in water was added and the mixture was extracted with DCM. The combined organic layers were dried (Na2SO4), filtered and evaporated to afford the title compound (132 mg). The crude product was used unpurified in the next step. UPLC: 0.56 min, MS: (ES/+) m/z: 327 [MH]+, C19H19FN2O2 requires 326.

후처리

  1. extractionthe mixture was extracted with DCM
  2. dry with materialThe combined organic layers were dried (Na2SO4)
  3. filtrationfiltered
  4. customevaporated

출처 및 근거

ORD 기록
ord-333b723a9ae144d3a1c7d2b9abc09990
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07855218B2

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