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Thiazole → HCID 22316611、化合物

HRID 2086645
ノート
印刷プレビュー

反応式

HRID 2086645 の反応式
[S:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[Li]CCCC.[CH3:11][C:12]1[N:13]([C:27]2[CH:32]=[CH:31][C:30](Br)=[CH:29][CH:28]=2)[C:14]([C:17]2[CH:22]=[CH:21][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:19][CH:18]=2)=[CH:15][CH:16]=1>CCOCC.C1COCC1.[Cl-].[Zn+2].[Cl-].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>[CH3:11][C:12]1[N:13]([C:27]2[CH:32]=[CH:31][C:30]([C:2]3[S:1][CH:5]=[CH:4][N:3]=3)=[CH:29][CH:28]=2)[C:14]([C:17]2[CH:18]=[CH:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=2)=[CH:15][CH:16]=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

8

反応物 3

HCID 9256ThiazoleHCID 223168431-(4-Bromophenyl)-2-methyl-5-[4-(methylsulfonyl)phenyl]-1H-pyrroleHCID 178418339Butyllithium

生成物 1

HCID 22316611HCID 22316611、化合物収率 13.2%

試薬・触媒・溶媒 4

HCID 3007855Zincchloride触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 3283Diethyl Ether溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

To a stirred solution of thiazole (0.072 g, 0.85 mmol) in anhydrous ether (2 mL) was added n-BuLi (0.58 mL, 1.61 M solution in hexane, 0.94 mmol) at −78° C. under nitrogen, the mixture was stirred for 30 minutes at −78° C., and then zinc chloride (2.55 mL, 1.0 M solution in ether, 2.55 mmol) was added at −78° C., the mixture was stirred for 30 minutes at −78° C. The reaction mixture was warmed to 0° C., and added the solution of 2-methyl 5-[4-(methylsulfonyl)phenyl]-1-(4-bromophenyl)-1H-pyrrole (0.3 g, 0.77 mmol) in THF (5 mL), tetrakis(triphenylphosphine)palladium (0) (0.088 g, 0.08 mmol). The reaction mixture was heated at reflux temperature for 19 hours, and cooled down to room temperature. The reaction mixture was filtered through celite, the filtrate was poured into water and the whole was extracted with ethyl acetate (20 mL×3). The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with hexane/ethyl acetate (2/1). The resulting solid was recrystallized from CH2Cl2/hexane to give the title compound (0.040 g, 13.2% yield).

後処理

  1. stirringthe mixture was stirred for 30 minutes at −78° C
  2. temperatureThe reaction mixture was warmed to 0° C.
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux temperature for 19 hours
  5. temperaturecooled down to room temperature
  6. filtrationThe reaction mixture was filtered through celite
  7. additionthe filtrate was poured into water
  8. extractionthe whole was extracted with ethyl acetate (20 mL×3)
  9. washThe organic layer was washed with brine
  10. dry with materialdried over Na2SO4
  11. concentrationconcentrated in vacuo
  12. customThe residue was purified by flash chromatography
  13. washeluting with hexane/ethyl acetate (2/1)
  14. customThe resulting solid was recrystallized from CH2Cl2/hexane

出典と根拠

ORDレコード
ord-a2c0d42e08ad4851830a34595e3bd4c1
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06727238B2

反応ノート

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