Methyl propiolate → HCID 86714138、化合物

HRID 919868

反応式

HRID 919868 の反応式
[CH2:1]([O:3][C:4](=[O:15])[CH:5]=[C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:7])[CH3:2].[CH3:16][O:17][C:18](=[O:21])[C:19]#[CH:20]>CO>[CH3:16][O:17][C:18](=[O:21])[CH:19]=[CH:20][C:5](=[C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:7])[C:4]([O:3][CH2:1][CH3:2])=[O:15]

参加物

4

反応物 2

HCID 13536Methyl propiolateHCID 94928Ethyl 3-anilinobut-2-enoate

生成物 1

HCID 86714138HCID 86714138、化合物収率 59.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 3-phenylamino-but-2-enoic acid ethyl ester (7 g, 34.1 mmol) and propynoic acid methyl ester (4.6 mL, 51.2 mmol) in MeOH (114 mL) was refluxed for 48 h. The solvent was evaporated, and the crude oil was purified by silica gel chromatography (0-20% EtOAc/hexanes) to give 5.88 g of the title compound as an orange oil. MS: (+) m/z 290.27 (M+1).

後処理

  1. temperaturewas refluxed for 48 h
  2. customThe solvent was evaporated
  3. customthe crude oil was purified by silica gel chromatography (0-20% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-ab242cb9833242d9af20b9f7b5f7cb71
出典データセット
uspto-grants-2016_03
特許番号
US09271970B2

関連ノート

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