Potassium Carbonate → HCID 66576591, 화합물

HRID 1405192노트

반응식

HRID 1405192 반응식
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][S:16]([CH3:19])(=[O:18])=[O:17])[CH:10]=2)[N:3]=1.[Cl:20][C:21]1[CH:26]=[CH:25][C:24](B(O)O)=[C:23]([O:30][CH:31]2[CH2:35][CH2:34][CH2:33][CH2:32]2)[CH:22]=1.C(=O)([O-])[O-].[K+].[K+]>COCCOC.C(OCC)(=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([C:2]2[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]3[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][S:16]([CH3:19])(=[O:18])=[O:17])[CH:10]=3)[N:3]=2)=[C:23]([O:30][CH:31]2[CH2:35][CH2:34][CH2:33][CH2:32]2)[CH:22]=1

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 219563434-chloro-N-{3-[(methylsulfonyl)methyl]phenyl}-1,3,5-triazin-2-amineHCID 53216478[4-Chloro-2-(cyclopentyloxy)phenyl]boronic acid

생성물 1

HCID 66576591HCID 66576591, 화합물

시약·촉매·용매 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 80711,2-Dimethoxyethane용매HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

A batch with crude crude 4-chloro-N-{3-[(methylsulfonyl)methyl]phenyl}-1,3,5-triazin-2-amine (175 mg), [4-chloro-2-(cyclopentyloxy)phenyl]boronic acid (141 mg; 0.59 mmol; Combi-Blocks Inc.) and [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride (72 mg; 0.09 mmol) in 1,2-dimethoxyethane (2.0 mL) and 2M solution of potassium carbonate (0.6 mL) was degassed using argon. The batch was stirred under argon for 60 minutes at 100° C. After cooling the batch was diluted with ethyl acetate. The organic phase was filtered using a Whatman filter and concentrated. The residue was purified by preparative HPLC.

후처리

  1. temperatureAfter cooling the batch
  2. filtrationThe organic phase was filtered
  3. filtrationfilter
  4. concentrationconcentrated
  5. customThe residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-21d4568740ff4bc0a104e5fa4bfc9e77
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916557B2

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