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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 5-(5-Bromo-2-chloropyrimidin-4-yl)-N-(4-fluorophenyl)thiazol-2-amine

HRID 2267390
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HRID 2267390 반응식
[Li]C(C)(C)C.[F:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14]2[S:15][CH:16]=[CH:17][N:18]=2)=[CH:9][CH:8]=1.[Br:19][C:20]1[CH:21]=[N:22][C:23]([Cl:26])=[N:24][CH:25]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl.O=C1O[C@H]([C@H](CO)O)C([O-])=C1O.[Na+]>CCCCCCC.C1COCC1.O.CO>[Br:19][C:20]1[C:21]([C:16]2[S:15][C:14]([NH:13][C:10]3[CH:9]=[CH:8][C:7]([F:6])=[CH:12][CH:11]=3)=[N:18][CH:17]=2)=[N:22][C:23]([Cl:26])=[N:24][CH:25]=1
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참가 물질

10

반응물 5

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 6066655-Bromo-2-chloropyrimidineHCID 23667548Sodium AscorbateHCID 25093329N-(4-Fluorophenyl)thiazol-2-amineHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 602045115-(5-Bromo-2-chloropyrimidin-4-yl)-N-(4-fluorophenyl)thiazol-2-amine

시약·촉매·용매 4

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8900Heptane용매

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온도
0 °C

실험 절차

8.1 mL (12 mmol) of a 1.5 M solution of tBuLi in heptane was added to a stirred solution of 1.1 g (5.5 mmol) of N-(4-fluorophenyl)thiazol-2-amine in 20 mL of THF at −20° C. The solution was stirred for 30 min and then cooled to −78° C. before 1.3 g (6.6 mmol) of 5-bromo-2-chloropyrimidine was added. The reaction solution was stirred for 30 min at −78° C., then quenched by addition of 0.2 mL of AcOH in 1 mL of MeOH. Solid 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (10.4 g, 46 mmol) and 5 mL of MeOH were added and the reaction solution was warmed to 0° C. and stirred for 30 min, poured into 50 mL of a 0.5 M solution of sodium ascorbate, diluted with 200 mL of water and the crude product removed by filtration and washed repeatedly with water. The crude product was purified by flash chromatography eluting with a linear gradient of 10% EtOAc in hexane to 80% EtOAc in hexane to deliver the desired compound. MS (M+H)+ 387.

후처리

  1. additionwas added
  2. stirringThe reaction solution was stirred for 30 min at −78° C.
  3. customquenched by addition of 0.2 mL of AcOH in 1 mL of MeOH
  4. stirringstirred for 30 min
  5. customthe crude product removed by filtration
  6. washwashed repeatedly with water
  7. customThe crude product was purified by flash chromatography
  8. washeluting with a linear gradient of 10% EtOAc in hexane to 80% EtOAc in hexane

출처 및 근거

ORD 기록
ord-b8f23b23c71a4e7abbe33b856fc0c3df
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858785B2

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