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Phosphoric Acid → 4-(2-Chloro-pyrido[2,3-d]pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester

HRID 1012946
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HRID 1012946 반응식
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[CH:11]=[CH:10][CH:9]=[N:8][C:6]=2[N:7]=1.NC1N=CC=CC=1C(O)=O.[C:23]([O:27][C:28]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)=[O:29])([CH3:26])([CH3:25])[CH3:24].CCN(C(C)C)C(C)C.P(=O)(O)(O)O>C(O)C.CO>[C:23]([O:27][C:28]([N:30]1[CH2:35][CH2:34][N:33]([C:4]2[C:5]3[CH:11]=[CH:10][CH:9]=[N:8][C:6]=3[N:7]=[C:2]([Cl:1])[N:3]=2)[CH2:32][CH2:31]1)=[O:29])([CH3:26])([CH3:24])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 1004Phosphoric AcidHCID 729302-Aminonicotinic acidHCID 81531DiisopropylethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 222222282,4-Dichloro-pyrido[2,3-d]pyrimidine

생성물 1

HCID 597321274-(2-Chloro-pyrido[2,3-d]pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester
수율 40%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

A mixture of 2,4-dichloro-pyrido[2,3-d]pyrimidine (150 mg, 0.75 mmol, 1 eq) [prepared from 2-aminonicotinic acid by the methods of Robins et al. (J. Am. Chem. Soc. 1955, 77, 1045.) and Oakes et al. (J. Chem. Soc. 1956, 1045.)], N-t-butoxycarbonyl piperazine (147 mg, 0.787 mmol, 1.05 eq) and Hunig's base (0.39 mL, 2.25 mmol, 3 eq) in ethanol (2.5 mL) was stirred at rt for 17 hr. The white solid was collected by filtration, washed with water and cold ethanol, and dried to afford C1.1 (105 mg, 40% yield). LC/MS: 350.41 [M+H]+; HPLC: >95% at 1.44 min (Xterra 5 μm C18 column 4.6×30 mm, 10-90% aqueous methanol over 2 min containing 0.2% phosphoric acid, 5 mL/min, monitoring at 254 nm).

후처리

  1. filtrationThe white solid was collected by filtration
  2. washwashed with water and cold ethanol
  3. customdried
  4. customto afford C1.1 (105 mg, 40% yield)

출처 및 근거

ORD 기록
ord-876a0a34330d467ca003e40da1d273aa
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981881B2

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