Triethylamine → HCID 59625986、化合物

HRID 468178ノート

反応式

HRID 468178 の反応式
[NH:1]1[CH2:4][CH:3]([N:5]2[CH2:10][CH2:9][N:8]([C:11]([C:13]3[S:14][CH:15]=[CH:16][N:17]=3)=[O:12])[CH2:7][CH2:6]2)[CH2:2]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC.[F:49][C:50]1[CH:55]=[CH:54][C:53]([N:56]2[C:60]3[CH:61]=[CH:62][C:63]([C:65](O)=[O:66])=[CH:64][C:59]=3[N:58]=[CH:57]2)=[CH:52][CH:51]=1>C(Cl)Cl.O>[F:49][C:50]1[CH:51]=[CH:52][C:53]([N:56]2[C:60]3[CH:61]=[CH:62][C:63]([C:65]([N:1]4[CH2:2][CH:3]([N:5]5[CH2:6][CH2:7][N:8]([C:11]([C:13]6[S:14][CH:15]=[CH:16][N:17]=6)=[O:12])[CH2:9][CH2:10]5)[CH2:4]4)=[O:66])=[CH:64][C:59]=3[N:58]=[CH:57]2)=[CH:54][CH:55]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 43566624HCID 43566624、化合物HCID 59625677(4-(Azetidin-3-yl)piperazin-1-yl)(thiazol-2-yl)methanone

生成物 1

HCID 59625986HCID 59625986、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5e (0.058 g, 0.178 mmol) and HATU (0.081 g, 0.214 mmol) in CH2Cl2 (3 mL) was added Et3N (0.099 mL, 0.713 mmol). The mixture was stirred at room temperature for 30 min, and then 60f (0.050 g, 0.196 mmol) was added. The reaction mixture was stirred at room temperature overnight. Water (6 mL) was added and the mixture was extracted with EtOAc. The organic layer was dried over MgSO4 and concentrated. The crude product Cpd 1167 was purified by preparative reverse phase chromatography. MS m/z (M+H+) 491.2.

後処理

  1. stirringThe reaction mixture was stirred at room temperature overnight
  2. extractionthe mixture was extracted with EtOAc
  3. dry with materialThe organic layer was dried over MgSO4
  4. concentrationconcentrated
  5. customThe crude product Cpd 1167 was purified by preparative reverse phase chromatography

出典と根拠

ORDレコード
ord-135bb3ed91d84cc3ae5e73cf985b1c7d
出典データセット
uspto-grants-2014_01
特許番号
US08623858B2

反応ノート

読み込み中…