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

HRID 1698528

반응식

HRID 1698528 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-749a808ba22c4faca68f4875942b2870
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163935B2

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