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Lithium Chloride → HCID 178519565, 화합물

HRID 2177600
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HRID 2177600 반응식
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][C:17]2[C:20](I)=[N:21][NH:22][C:16]=2[CH2:15]1)=[O:13].ClC1C(C(F)(F)F)=CC=CC=1C([N:37]1CCC2C(I)=N[N:45]([CH:46]3[CH2:51]CCCO3)[C:39]=2[CH2:38]1)=O.C([Sn](CCCC)(CCCC)C1C=NC=CN=1)CCC.[Cl-].[Li+]>O1CCOCC1.O.CCOC(C)=O.[F-].[K+].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][C:17]2=[C:20]([C:39]3[CH:38]=[N:37][CH:51]=[CH:46][N:45]=3)[NH:21][N:22]=[C:16]2[CH2:15]1)=[O:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 433294Lithium ChlorideHCID 27373162-(Tributylstannyl)pyrazineHCID 90409002HCID 90409002, 화합물HCID 90409420HCID 90409420, 화합물

생성물 1

HCID 178519565HCID 178519565, 화합물

시약·촉매·용매 5

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매
HCID 312751,4-Dioxane용매
HCID 522689Potassium Fluoride용매

반응 조건

온도
170 °C

실험 절차

To a solution of 6-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-3-iodo-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine (Intermediate 57) (47 mg, 0.103 mmol) in 1,4-dioxane (1 mL) was added 2-tributylstannylpyrazine (0.041 mL, 0.124 mmol), lithium chloride (4 mg, 0.103 mmol) and tetrakis(triphenylphosphine)palladium(0) (119 mg, 0.103 mmol). The reaction was allowed to stir overnight at 110° C. and an additional 3 h in a microwave reactor at 170° C. The reaction was diluted with water and EtOAc and 50% potassium fluoride on Celite© (1 g) was added. After stirring for 1 h, the solution was filtered and the layers in the filtrate were separated. The organic layer was concentrated in vacuo and the residue was purified by HPLC (Agilent prep system, Waters XBridge, C18, 5 μm, 30×100 mm column, 5-99% MeOH/20 mM NH4OH over 18 min at 30 mL/min) to give the desired product. (3 mg, 8%). MS (ESI) mass calcd. C18H13ClF3N5O, 407.1. m/z found 408.1 [M+H]+. 1H NMR (500 MHz, CDCl3) δ 8.88 (br s, 1H), 8.60-8.50 (m, 2H), 7.82-7.75 (m, 1H), 7.57-7.41 (m, 3H), 5.20-5.13 (m, 0.5H), 4.95-4.87 (m, 0.5H), 4.52 (d, J=15.7 Hz, 0.5H), 4.41 (d, J=15.8 Hz, 0.5H), 4.34-4.27 (m, 0.5H), 4.10-3.97 (m, 0.5H), 3.60-3.53 (m, 1H), 3.16-3.12 (m, 1H), 2.98 (m, 1H).

후처리

  1. additionwas added
  2. stirringAfter stirring for 1 h
  3. filtrationthe solution was filtered
  4. customthe layers in the filtrate were separated
  5. concentrationThe organic layer was concentrated in vacuo
  6. customthe residue was purified by HPLC (Agilent prep system, Waters XBridge, C18, 5 μm, 30×100 mm column, 5-99% MeOH/20 mM NH4OH over 18 min at 30 mL/min)

출처 및 근거

ORD 기록
ord-71885764873d4c86b75f4843e7d9b1fd
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09066946B2

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