Ethyl propiolate → HCID 59252478、化合物

HRID 237886ノート

反応式

HRID 237886 の反応式
[CH:1]1([C:7]2[CH:12]=[CH:11][C:10]([NH:13][CH2:14][CH:15]3[O:19][C:18]([NH2:20])=[N:17][CH2:16]3)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:21](OCC)(=[O:24])[C:22]#[CH:23]>C(O)C>[CH:1]1([C:7]2[CH:12]=[CH:11][C:10]([NH:13][CH2:14][CH:15]3[O:19][C:18]4=[N:20][C:21](=[O:24])[CH:22]=[CH:23][N:17]4[CH2:16]3)=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 12182Ethyl propiolateHCID 68529232HCID 68529232、化合物

生成物 1

HCID 59252478HCID 59252478、化合物収率 217.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 5-[(4-cyclohexyl-phenylamino)-methyl]-4,5-dihydro-oxazol-2-ylamine (1.13 g, 4.14 mmol) in 50 ml of ethanol was added 0.42 ml (0.415 mmol) of ethyl propiolate. The mixture was stirred at reflux for 6 h under nitrogen after which it was allowed to cool to room temperature. The resulting white crystals were isolated by filtration, washed with ethanol, and dried at room temperature under high vacuum to provide 0.294 g of the title compound. The filtrate from the filtration was concentrated to 10 ml and allowed to stand for 6 h. The resulting white crystals were isolated by filtration and dried under high vacuum to provide an additional 0.059 g of the title compound.

後処理

  1. temperatureat reflux for 6 h under nitrogen after which it
  2. customThe resulting white crystals were isolated by filtration
  3. washwashed with ethanol
  4. customdried at room temperature under high vacuum

出典と根拠

ORDレコード
ord-4b4a5d165c764e05a5fcb78aa7c54a33
出典データセット
uspto-grants-2014_02
特許番号
US08642603B2

反応ノート

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