N,N-Dimethylethylenediamine → HCID 59333652, 화합물

HRID 1876517노트

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HRID 1876517 반응식
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH2:5].Cl[C:8]1[N:9]([CH2:31][CH:32]2[CH2:34][CH2:33]2)[C:10]2[C:15]([N:16]=1)=[C:14]([N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1)[N:13]=[C:12]([C:23]1[C:24]([CH3:30])=[N:25][C:26]([NH2:29])=[N:27][CH:28]=1)[N:11]=2>CS(C)=O>[NH2:29][C:26]1[N:25]=[C:24]([CH3:30])[C:23]([C:12]2[N:11]=[C:10]3[C:15]([N:16]=[C:8]([NH:5][CH2:4][CH2:3][N:2]([CH3:6])[CH3:1])[N:9]3[CH2:31][CH:32]3[CH2:34][CH2:33]3)=[C:14]([N:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)[N:13]=2)=[CH:28][N:27]=1

참가 물질

4

반응물 2

HCID 66053N,N-DimethylethylenediamineHCID 593334985-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine

생성물 1

HCID 59333652HCID 59333652, 화합물수율 54.4%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
150 °C

실험 절차

N,N-Dimethylethylenediamine (110 mg, 1.3 mmol) and dimethyl sulfoxide (700 μl) were added to 5-[8-chloro-9-(cyclopropylmethyl)-6-morpholin-4-yl-9H-purin-2-yl]-4-methylpyrimidin-2-amine (100 mg, 0.26 mmol) and the resulting mixture was stirred at 150° C. for 3 hours. The reaction mixture was partitioned with ethyl acetate and water, the organic layer was concentrated, and then the residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid) to give the title compound (64 mg, 52%) as a pale yellow solid.

후처리

  1. customThe reaction mixture was partitioned with ethyl acetate and water
  2. concentrationthe organic layer was concentrated
  3. customthe residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)

출처 및 근거

ORD 기록
ord-a2b6912be6ef41e2abac66de93d77cc0
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309546B2

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