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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
ノート
印刷プレビュー

反応式

HRID 2267390 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 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、化合物

生成物 1

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

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8900Heptane溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b8f23b23c71a4e7abbe33b856fc0c3df
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858785B2

反応ノート

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