Chloroform → HCID 18536748、化合物

HRID 412078

反応式

HRID 412078 の反応式
CC(C)([O-])C.[K+].[F:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]=1[C:17]([F:20])([F:19])[F:18].[CH:21](Cl)([Cl:23])[Cl:22].C(O)(=O)C.CO>O1CCCC1.[Cl-].[Na+].O.CCCCCC.C(OCC)(=O)C>[Cl:22][CH:21]([Cl:23])[C:12]1[C:11]([N+:14]([O-:16])=[O:15])=[CH:10][C:9]([C:17]([F:18])([F:19])[F:20])=[C:8]([F:7])[CH:13]=1

参加物

9

反応物 4

HCID 6212ChloroformHCID 949542-Fluoro-5-nitrobenzotrifluorideHCID 10129899Acetic acid methanolHCID 23665647Potassium tert-butoxide

生成物 1

HCID 18536748HCID 18536748、化合物収率 51.2%

試薬・触媒・溶媒 4

HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

To a solution of potassium t-butoxide (1.25 g, 11.1 mmol) in tetrahydrofuran (25 ml) was slowly added dropwise a solution of 2-fluoro-5-nitrobenzotrifluoride (1.00 g, 4.78 mmol) and chloroform (599 mg, 5.02 mmol) in tetrahydrofuran (2.5 ml) at −78° C. After stirring for 15 minutes at the same temperature, acetic acid-methanol (1:1, 5 ml) was added and the temperature was raised to room temperature. Ethyl acetate and saturated brine were added to the reaction mixture, which was extracted with ethyl acetate. After washed with brine, the organic layer was dried over anhydrous magnesium sulfate and solvent was distilled off. The residue obtained was submitted to silica gel column chromatography [hexane→hexane-ethyl acetate(300:1)] to obtain 714 mg of title compound as pale yellow liquid. Yield 51%.

後処理

  1. additionwas added
  2. extractionwas extracted with ethyl acetate
  3. washAfter washed with brine
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate and solvent
  5. distillationwas distilled off
  6. customThe residue obtained

出典と根拠

ORDレコード
ord-709a237c3984425b80c000aa069b163e
出典データセット
uspto-grants-2003_05
特許番号
US06562839B1

関連ノート

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