Diisopropylethylamine → HCID 90017038, 화합물

HRID 1055003노트

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HRID 1055003 반응식
[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][C:9]([OH:11])=O)=[N:5][C:4]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)=[N:3]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C.[CH2:50]([C:52]1[C:53]([NH:59][NH2:60])=[N:54][C:55]([CH3:58])=[N:56][CH:57]=1)[CH3:51]>CN(C)C=O>[CH2:50]([C:52]1[C:53]([NH:59][NH:60][C:9](=[O:11])[CH2:8][CH2:7][C:6]2[N:2]([CH3:1])[N:3]=[C:4]([N:12]3[CH2:16][CH2:15][CH2:14][CH2:13]3)[N:5]=2)=[N:54][C:55]([CH3:58])=[N:56][CH:57]=1)[CH3:51]

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 83891736HCID 83891736, 화합물HCID 90016952HCID 90016952, 화합물

생성물 1

HCID 90017038HCID 90017038, 화합물수율 31.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-(1-Methyl-3-(pyrrolidin-1-yl)-1H-1,2,4-triazol-5-yl)propanoic acid (140 mg, 0.624 mmol), HATU (712 mg, 1.87 mmol) and N,N-diisopropylethylamine (600 μl, 3.53 mmol) were dissolved in dimethylformamide (18 mL). The mixture was stirred for 20 minutes. 5-Ethyl-4-hydrazinyl-2-methylpyrimidine (99 mg, 0.655 mmol) was added and the reaction mixture was allowed to stir at room temperature overnight. The mixture was concentrated to an oil. Preparative HPLC afforded the desired product (71 mg, 31%) as a yellow gum. MS: m/z=359.23 (M+H+)

후처리

  1. stirringto stir at room temperature overnight
  2. concentrationThe mixture was concentrated to an oil

출처 및 근거

ORD 기록
ord-d44a75693d2d43e09f9ea0eda6a18c1d
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394311B2

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