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Triethylamine → (E)-1-[4-(2,6-Dimethoxy-4-pyridyl)piperazin-1-yl]-4,4,5,5,5-pentafluoro-pent-2-en-1-one

HRID 333956
ノート
印刷プレビュー

反応式

HRID 333956 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[C:5]([O:15][CH3:16])[N:4]=1.[F:17][C:18]([F:28])([C:24]([F:27])([F:26])[F:25])/[CH:19]=[CH:20]/[C:21](O)=[O:22].C(N(CC)CC)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:9]2[CH2:10][CH2:11][N:12]([C:21](=[O:22])/[CH:20]=[CH:19]/[C:18]([F:17])([F:28])[C:24]([F:25])([F:26])[F:27])[CH2:13][CH2:14]2)[CH:6]=[C:5]([O:15][CH3:16])[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 668358261-(2,6-Dimethoxy-4-pyridyl)piperazineHCID 86691160(2E)-4,4,5,5,5-Pentafluoro-2-pentenoic acid

生成物 1

HCID 86691597(E)-1-[4-(2,6-Dimethoxy-4-pyridyl)piperazin-1-yl]-4,4,5,5,5-pentafluoro-pent-2-en-1-one
収率 17.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-(2,6-Dimethoxy-4-pyridyl)piperazine (30 mg, 0.13 mmol) was dissolved in anhydrous dichloromethane (2 ml) together with (E)-4,4,5,5,5-pentafluoropent-2-enoic acid (35 mg, 0.18 mmol), triethylamine (31 mg, 44 μl, 0.32 mmol), HBTU (74 mg, 0.15 mmol) and stirred at room temperature for two hours. The mixture was evaporated to dryness under reduced pressure and the residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 9 mg of a solid (0.023 mmol, 15%).

後処理

  1. customThe mixture was evaporated to dryness under reduced pressure
  2. customthe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)

出典と根拠

ORDレコード
ord-8dc5061ba248457db9fa847e4f5dbac1
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883791B2

反応ノート

読み込み中…

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