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Diisopropylethylamine → HCID 21081017, 화합물

HRID 2380826
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HRID 2380826 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([O:9][CH3:10])=[CH:4][N:3]=1.Cl.Cl.[NH:13]1[C:17]2[CH2:18][CH2:19][CH2:20][NH:21][C:16]=2[N:15]=[CH:14]1.C(N(C(C)C)C(C)C)C>C(O)CCC>[Cl:1][C:2]1[N:7]=[C:6]([N:21]2[CH2:20][CH2:19][C:18]3[N:15]=[CH:14][NH:13][C:17]=3[CH2:16]2)[C:5]([O:9][CH3:10])=[CH:4][N:3]=1
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 6014012,4-Dichloro-5-methoxypyrimidineHCID 68845019HCID 68845019, 화합물

생성물 1

HCID 21081017HCID 21081017, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
50 °C

실험 절차

1 g 2,4-dichloro-5-methoxy-pyrimidine are dissolved in 4 mL butanol and combined with 1.04 g 4,5,6,7-tetrahydroimidazopyridine dihydrochloride and 2.96 mL ethyldiisopropylamine. This mixture is stirred for 16 h at 50° C. and then the solvent is eliminated in vacuo. The crude mixture is purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which consists at the starting point of 95% water and 5% acetonitrile and at the finishing point of 70% water and 30% acetonitrile. 0.2% formic acid is added to both eluants. The suitable fractions are freeze-dried.

후처리

  1. customThe crude mixture is purified by column chromatography
  2. addition0.2% formic acid is added to both eluants
  3. customThe suitable fractions are freeze-dried

출처 및 근거

ORD 기록
ord-bbe8789f04bc4773a5970af04c4b6545
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08258129B2

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