Methylamine → (S)-N-Methylhydroxysuccinimide

HRID 364371노트

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HRID 364371 반응식
[C:1]([OH:9])(=O)[C@H:2]([CH2:4][C:5](O)=[O:6])[OH:3].[CH3:10][NH2:11]>C1(C)C=CC=CC=1>[OH:3][C@H:2]1[CH2:4][C:5](=[O:6])[N:11]([CH3:10])[C:1]1=[O:9]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 222656L-Malic Acid

생성물 1

HCID 13726417(S)-N-Methylhydroxysuccinimide

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirred solution of 134 g (1 mole) of (S)-malic acid in 700 ml of toluene was added 97 ml of 40% aqueous methylamine. The temperature slowly rose to 50° C. After 0.5 hr the stirred mixture was heated to reflux and the water was collected in a Dean-Stark trap for 48 hr. A total of 93 ml of water was collected. The toluene residue was treated with 300 ml of ethanol and concentrated on the rotary evaporator. The residue was distilled. The yield of product obtained was 101 g (78%), b.p. 140°/2 mm; 145°/0.5 mm.

후처리

  1. customslowly rose to 50° C
  2. temperatureAfter 0.5 hr the stirred mixture was heated
  3. temperatureto reflux
  4. customthe water was collected in a Dean-Stark trap for 48 hr
  5. customA total of 93 ml of water was collected
  6. additionThe toluene residue was treated with 300 ml of ethanol
  7. concentrationconcentrated on the rotary evaporator
  8. distillationThe residue was distilled
  9. customThe yield of product obtained
  10. custom145°/0.5 mm

출처 및 근거

ORD 기록
ord-ee2873bab3004c9c8698d04697638ff1
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04604388

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