1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 57691340、化合物

HRID 219083

反応式

HRID 219083 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][N:10]3[N:13]=[N:14][C:15]([C:16]([O-:18])=O)=[C:9]3[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1([C:25]2[CH:30]=[CH:29][N:28]=[C:27]([CH2:31][C:32]([O:34][CH3:35])=O)[CH:26]=2)C=CC=CC=1.[CH2:36]1CCN2C(=NCCC2)C[CH2:37]1.C(NC1C=CC(S(N=[N+]=[N-])(=O)=O)=CC=1)(=O)C>CC#N>[CH3:35][O:34][C:32]1[CH:31]=[C:27]2[C:26]([C:25]([O:18][CH2:16][C:15]3[N:14]=[N:13][N:10]4[CH:11]=[CH:12][C:7]([C:1]5[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=5)=[CH:8][C:9]=34)=[CH:30][CH:29]=[N:28]2)=[CH:37][CH:36]=1

参加物

6

反応物 4

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 51291854-Acetamidobenzenesulfonyl azideHCID 67503470HCID 67503470、化合物HCID 86630264HCID 86630264、化合物

生成物 1

HCID 57691340HCID 57691340、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

5-Phenyl-[1,2,3]triazolo[1,5-a]pyridine-3-carboxylate. To a solution of methyl 2-(4-phenylpyridin-2-yl)acetate (see Lohse, O.; Thevenin, P.; Waldvogel, E. Synlett 1999, 1, 45-48) (0.504 g, 2.22 mmol) in 12 mL CH3CN was added DBU (0.501 ml, 3.33 mmol) and the mixture cooled in an ice bath. To the solution, 4-acetamidobenzenesulfonyl azide (0.533 g, 2.22 mmol) was added and the mixture allowed to warm to rt. The mixture was stirred at rt for 5 h then evaporated. The residue was diluted with CH2Cl2, washed with water, brine, dried over Na2SO4, and filtered. The title compound was obtained after purification via flash chromatography.

後処理

  1. temperaturethe mixture cooled in an ice bath
  2. customthen evaporated
  3. additionThe residue was diluted with CH2Cl2
  4. washwashed with water, brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-9777b9de91304c46a43ed3a49353da7b
出典データセット
uspto-grants-2012_06
特許番号
US08198448B2

関連ノート

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