Methylamine → Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester

HRID 1698528

反応式

HRID 1698528 の反応式
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH3:15][NH2:16]>O1CCCC1>[CH3:15][NH:16][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

参加物

4

反応物 2

HCID 6329MethylamineHCID 10751184Methyl 2-chloro-3-nitrobenzoate

生成物 1

HCID 59635415Benzoic acid, 2-(methylamino)-3-nitro-, methyl ester収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 21.5 g (99.5 mmol) of methyl 2-chloro-3-nitrobenzoate in 300 mL of tetrahydrofuran (THF) was treated with drop wise addition of 300 mL (597 mmol) of methylamine (2M solution in THF) and was stirred overnight at room temperature. The reaction was concentrated to dryness, dissolved in dichloromethane, and washed with aqueous sodium bicarbonate and water. The organics were dried over sodium sulfate, filtered, and concentrated in vacuo to give 20.8 g (100%) of the title compound.

後処理

  1. concentrationThe reaction was concentrated to dryness
  2. dissolutiondissolved in dichloromethane
  3. washwashed with aqueous sodium bicarbonate and water
  4. dry with materialThe organics were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-749a808ba22c4faca68f4875942b2870
出典データセット
uspto-grants-2012_04
特許番号
US08163935B2

関連ノート

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