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1,1'-Carbonyldiimidazole → HCID 59654362、化合物

HRID 2053049
ノート
印刷プレビュー

反応式

HRID 2053049 の反応式
[F:1][C:2]([F:20])([F:19])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=1)[C:13](O)=[O:14].C(N1C=CN=C1)([N:23]1C=CN=C1)=O.C([O-])(=O)C.[NH4+]>CN(C=O)C>[F:1][C:2]([F:20])([F:19])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=1)[C:13]([NH2:23])=[O:14]
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 682631,1'-CarbonyldiimidazoleHCID 517165Ammonium AcetateHCID 167687772'-(Trifluoromethoxy)[1,1'-biphenyl]-3-carboxylic acid

生成物 1

HCID 59654362HCID 59654362、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 0.94 g (3.36 mmol) of 3-(2-trifluoromethoxyphenyl)-benzoic acid in 17 Ml of DMF was added 0.55 g (3.36 mmol) of carbonyldiimidazole (CDI) and the reaction was stirred at RT for 4 h. To the reaction mixture was added. 2.6 g (33.6 mmol) of ammonium acetate and the reaction mixture was stirred over night at RT. The reaction mixture was partitioned between ethyl acetate and water and the organic fraction was washed with brine, dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by chromatography (silica, 30%, 50% successively EtOAc: hexanes) to give the title compound. Mass Spectrum (ESI) m/e (M+1): 282.2.

後処理

  1. additionTo the reaction mixture was added
  2. customThe reaction mixture was partitioned between ethyl acetate and water
  3. washthe organic fraction was washed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated
  7. customThe residue was purified by chromatography (silica, 30%, 50% successively EtOAc

出典と根拠

ORDレコード
ord-b119c5d289be4d45800480ba15743547
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07326726B2

反応ノート

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