Hydrogen Sulfide → Methyl 1-methylpyrrol-2-acetate

HRID 1703752노트

반응식

HRID 1703752 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=O)[C:8]([O:10][CH3:11])=[O:9].S>N1C=CC=CC=1>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH2:7][C:8]([O:10][CH3:11])=[O:9]

참가 물질

4

반응물 2

HCID 402Hydrogen Sulfide2회HCID 22759895Methyl 1-methyl-α-oxo-1H-pyrrole-2-acetate

생성물 1

HCID 103992Methyl 1-methylpyrrol-2-acetate수율 86%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
63 °C

실험 절차

A solution of 50g of methyl 1-methylpyrrole-2-glyoxylate in 200 ml of pyridine is cooled to -78° C. and 64g of hydrogen sulfide is added. The mixture is sealed in a stirred autoclave and heated to 63° C. The pressure rises to about 130 p.s.i. After 27 hrs., the hydrogen sulfide is driven off in a nitrogen stream and the solution is decanted from the precipitated sulfur. Pyridine is distilled off at 20 mm Hg. The residue is distilled at 0.03 mm Hg, b.p. 68-70° C., to give 39.2g of oily methyl 1-methylpyrrole-2-acetate (86% yield).

후처리

  1. customThe mixture is sealed in a stirred autoclave
  2. customthe solution is decanted from the precipitated sulfur
  3. distillationPyridine is distilled off at 20 mm Hg
  4. distillationThe residue is distilled at 0.03 mm Hg, b.p. 68-70° C.

출처 및 근거

ORD 기록
ord-fc05f2eb207c43fca3530064e22b3743
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04125537

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