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Dichloromethane → 3-(3-Chlorophenyl)-2,6-dimethylthieno[2,3-b]pyridin-4-amine

HRID 573543
ノート
印刷プレビュー

反応式

HRID 573543 の反応式
Br[C:2]1[C:10]2[C:9]([NH2:11])=[CH:8][C:7]([CH3:12])=[N:6][C:5]=2[S:4][C:3]=1[CH3:13].[Cl:14][C:15]1[CH:16]=[C:17](B(O)O)[CH:18]=[CH:19][CH:20]=1.C(Cl)Cl.C([O-])([O-])=O.[Cs+].[Cs+]>C1(C)C=CC=CC=1.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].O>[Cl:14][C:15]1[CH:20]=[C:19]([C:2]2[C:10]3[C:9]([NH2:11])=[CH:8][C:7]([CH3:12])=[N:6][C:5]=3[S:4][C:3]=2[CH3:13])[CH:18]=[CH:17][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 4

HCID 6344DichloromethaneHCID 10796Cesium carbonateHCID 2734323(3-Chlorophenyl)boronic acidHCID 683238623-Bromo-2,6-dimethylthieno[2,3-b]pyridin-4-amine

生成物 1

HCID 683240173-(3-Chlorophenyl)-2,6-dimethylthieno[2,3-b]pyridin-4-amine収率 107.1%

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
150 °C

実験手順

Under nitrogen, 3-bromo-2,6-dimethylthieno[2,3-b]pyridin-4-amine (170 mg, 0.661 mmol) (Description 8) was dissolved in toluene (6 mL) and (3-chlorophenyl)boronic acid (155 mg, 0.992 mmol), PdCl2(dppf).DCM (54.0 mg, 0.066 mmol) and Cs2CO3 (646 mg, 1.983 mmol) were added and the mixture heated in a microwave at 150° C. for 30 min. The reaction mixture was combined with the material (30 mg) from similar reaction. Water (20 mL) was added and the mixture extracted with ethyl acetate (3×15 mL). The organic layer was dried over MgSO4, filtered and solvent removed in vacuo. Purification by chromatography on silica gel, eluting with a gradient of 0-50% ethyl acetate in cyclohexane, afforded the title compound (204.4 mg). LCMS (A) m/z: 291 [M+1]+, Rt 0.84 min (acidic).

後処理

  1. extractionthe mixture extracted with ethyl acetate (3×15 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customsolvent removed in vacuo
  5. customPurification by chromatography on silica gel
  6. washeluting with a gradient of 0-50% ethyl acetate in cyclohexane

出典と根拠

ORDレコード
ord-a16e56a030414cecbdba2da572508c5e
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09029545B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート