Methanol → AC-Pro-ome

HRID 579824

反応式

HRID 579824 の反応式
CC1C=CC=C(C)C=1C.C[OH:11].[C:12]([N:15]1[CH2:19][CH2:18][CH:17]=[CH:16]1)(=[O:14])[CH3:13].[O:20]1[CH2:24]CC[CH2:21]1>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:21][O:20][C:24](=[O:11])[C@@H:16]1[CH2:17][CH2:18][CH2:19][N:15]1[C:12](=[O:14])[CH3:13]

参加物

6

反応物 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 106861,2,3-TrimethylbenzeneHCID 10909522N-Acetyl-2-pyrroline2 回

生成物 1

HCID 11019314AC-Pro-ome収率 47.9%

試薬・触媒・溶媒 1

HCID 178418476HCID 178418476、化合物触媒

反応条件

温度
100 °C

実験手順

A 70 mL stainless steel high pressure reactor having a Pyrex glass liner and a magnetic stir bar was charged with 5 mL of tetrahydrofuran, 0.5 mmol of 1,2,3-trimethylbenzene internal standard, 0.6 mmol of CH3OH, 35.1 mg of (PPh3)2PdCl2, and 55.5 mg of N-acetyl-2-pyrroline. The reactor ws pressurized to 1000 psi with CO at room temperature, and the reaction mixture was stirred for 44.25 hours at 100° C. Thereafter, the reactor was cooled to room temperature and vented to atmospheric pressure. The product mixture was analyzed by gas chromatography and mass spectroscopy, and the analysis indicated complete conversion of N-acetyl-2-pyrroline and a 47.9% yield of N-acetylproline methyl ester.

後処理

  1. customA 70 mL stainless steel high pressure reactor having
  2. customws pressurized to 1000 psi with CO at room temperature
  3. temperatureThereafter, the reactor was cooled to room temperature

出典と根拠

ORDレコード
ord-db92a17fba884a99a405b18ab16d2606
出典データセット
uspto-grants-1988_06
特許番号
US04749786

関連ノート

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