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Trifluoroacetic acid → N-{4-[4-(4-chlorophenyl)-4,5,6,7-tetrahydro-1-benzothien-2-yl]pyridin-2-yl}acetamide

HRID 1615490
ノート
印刷プレビュー

反応式

HRID 1615490 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2(O)[C:13]3[CH:14]=[C:15]([C:17]4[CH:22]=[CH:21][N:20]=[C:19]([NH:23][C:24](=[O:26])[CH3:25])[CH:18]=4)[S:16][C:12]=3[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>ClCCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[C:13]3[CH:14]=[C:15]([C:17]4[CH:22]=[CH:21][N:20]=[C:19]([NH:23][C:24](=[O:26])[CH3:25])[CH:18]=4)[S:16][C:12]=3[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 68182981N-{4-[4-(4-chlorophenyl)-4-hydroxy-4,5,6,7-tetrahydro-1-benzothien-2-yl]pyridin-2-yl}acetamide

生成物 1

HCID 68183050N-{4-[4-(4-chlorophenyl)-4,5,6,7-tetrahydro-1-benzothien-2-yl]pyridin-2-yl}acetamide

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

In a 100 mL round bottomed flask was placed crude N-{4-[4-(4-chlorophenyl)-4-hydroxy-4,5,6,7-tetrahydro-1-benzothien-2-yl]pyridin-2-yl}acetamide (410 mg, 1.0 mmol) prepared above and 1,2-dichloroethane (10 mL). The mixture was refluxed for 30 min to obtain a yellow solution. To the refluxing mixture were added triethylsilane (1 mL, 6 mmol) and trifluoroacetic acid (2 mL, 20 mmol), and refluxing was continued for an additional 3 hr. The mixture was allowed to cool to rt then concentrated under reduced pressure. The residue was diluted with EtOAc (50 mL) then washed with a saturated aqueous solution of NaHCO3 (50 mL). The aqueous phase was extracted with EtOAc (50 mL). The combined organic phases were dried over anhydrous MgSO4.

後処理

  1. customIn a 100 mL round bottomed flask was placed
  2. temperatureThe mixture was refluxed for 30 min
  3. customto obtain a yellow solution
  4. temperaturerefluxing
  5. concentrationthen concentrated under reduced pressure
  6. additionThe residue was diluted with EtOAc (50 mL)
  7. washthen washed with a saturated aqueous solution of NaHCO3 (50 mL)
  8. extractionThe aqueous phase was extracted with EtOAc (50 mL)
  9. dry with materialThe combined organic phases were dried over anhydrous MgSO4

出典と根拠

ORDレコード
ord-e71ac04f0906441abc1c0b88cfed5a3b
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765746B2

反応ノート

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