Triethylamine → HCID 59625986, 화합물

HRID 468178노트

반응식

HRID 468178 반응식
[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

참가 물질

7

반응물 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, 화합물HCID 59625677(4-(Azetidin-3-yl)piperazin-1-yl)(thiazol-2-yl)methanone

생성물 1

HCID 59625986HCID 59625986, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-135bb3ed91d84cc3ae5e73cf985b1c7d
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623858B2

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