Hydrogen Sulfide → Methyl 1-methylpyrrol-2-acetate

HRID 1703752ノート

反応式

HRID 1703752 の反応式
[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]

参加物

4

反応物 2

HCID 402Hydrogen Sulfide2 回HCID 22759895Methyl 1-methyl-α-oxo-1H-pyrrole-2-acetate

生成物 1

HCID 103992Methyl 1-methylpyrrol-2-acetate収率 86%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
63 °C

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-fc05f2eb207c43fca3530064e22b3743
出典データセット
uspto-grants-1978_11
特許番号
US04125537

反応ノート

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