Diisopropylethylamine → HCID 90017038、化合物

HRID 1055003ノート

反応式

HRID 1055003 の反応式
[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]

参加物

6

反応物 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、化合物HCID 90016952HCID 90016952、化合物

生成物 1

HCID 90017038HCID 90017038、化合物収率 31.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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+)

後処理

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

出典と根拠

ORDレコード
ord-d44a75693d2d43e09f9ea0eda6a18c1d
出典データセット
uspto-grants-2016_07
特許番号
US09394311B2

反応ノート

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