Ethanol → Ethyl 5-chloro-2-nitrobenzoate

HRID 494410

反応式

HRID 494410 の反応式
[CH2:1]([OH:3])[CH3:2].C(N(CC)CC)C.[Cl:11][C:12]1[CH:13]=[CH:14][C:15]([N+:21]([O-:23])=[O:22])=[C:16]([CH:20]=1)[C:17](Cl)=[O:18].O>O1CCCC1.C(OCC)(=O)C>[CH2:1]([O:3][C:17](=[O:18])[C:16]1[CH:20]=[C:12]([Cl:11])[CH:13]=[CH:14][C:15]=1[N+:21]([O-:23])=[O:22])[CH3:2]

参加物

7

反応物 4

HCID 702EthanolHCID 962WaterHCID 8471TriethylamineHCID 27236855-Chloro-2-nitrobenzoyl chloride

生成物 1

HCID 603450Ethyl 5-chloro-2-nitrobenzoate

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of ethanol (1.23 mL), triethylamine (3.05 mL) and tetrahydrofuran (35 mL) was dropwise added a solution of 5-chloro-2-nitrobenzoic acid chloride (4.44 g) obtained in Example 9-4a) in tetrahydrofuran (10 mL) under ice-cooling. The mixture was stirred at room temperature overnight, and water was then added. The solution was diluted with ethyl acetate, and the organic layer was washed successively with saturated aqueous sodium bicarbonate and saturated brine, dried over sodium sulfate and concentrated to give the title compound (4.43 g) as a pale brown solid.

後処理

  1. temperaturecooling
  2. washthe organic layer was washed successively with saturated aqueous sodium bicarbonate and saturated brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-bcc03612ef434abd9353db96477337bc
出典データセット
uspto-grants-2009_05
特許番号
US07538140B2

関連ノート

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