Water → HCID 57990307, 화합물

HRID 2381639노트

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HRID 2381639 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[C:10]([I:11])=[CH:9][N:8]([S:12]([C:15]3[CH:21]=[CH:20][C:18]([CH3:19])=[CH:17][CH:16]=3)(=[O:14])=[O:13])[C:6]=2[N:7]=1.Cl.[C:24]([N:31]1[CH2:36][CH2:35][CH:34]([CH2:37][NH2:38])[CH2:33][CH2:32]1)([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25].O.CCOC(C)=O>CC#N>[Cl:1][C:2]1[N:3]=[C:4]([NH:38][CH2:37][CH:34]2[CH2:35][CH2:36][N:31]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:32][CH2:33]2)[C:5]2[C:10]([I:11])=[CH:9][N:8]([S:12]([C:15]3[CH:21]=[CH:20][C:18]([CH3:19])=[CH:17][CH:16]=3)(=[O:14])=[O:13])[C:6]=2[N:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 2756034tert-Butyl 4-(aminomethyl)piperidine-1-carboxylate--hydrogen chloride (1/1)HCID 579902932,4-dichloro-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 57990307HCID 57990307, 화합물수율 100%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2,4-dichloro-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine (244 mg, 0.520 mmol), 1-N—BOC-4-aminomethyl piperidine hydrochloride (130 mg, 0.520 mmol) and TEA (0.200 mL, 1.44 mmol) in CH3CN (6 mL) was stirred at room temperature for 16 h. Water and EtOAc were added. The organic phase was separated, washed with 1N HCl, then with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo to give tert-butyl 4-((2-chloro-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)methyl)piperidine-1-carboxylate (336 mg).

후처리

  1. customThe organic phase was separated
  2. washwashed with 1N HCl
  3. dry with materialwith 5% NaHCO3, dried over Na2SO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0246b4de5d264f21b2768cbb1de95528
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258144B2

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