Methane → HCID 69934936、化合物

HRID 380717ノート

反応式

HRID 380717 の反応式
[C:1]([O:11][C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][C:13]=1[N+:21]([O-])=O)(=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C>[Fe].O1CCOCC1>[C:1]([O:11][C:12]1[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][C:13]=1[NH2:21])(=[O:10])[CH:2]=[CH:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 2

HCID 297MethaneHCID 740530652-Propenoic acid, 3-phenyl-, 2,4-dinitrophenyl ester

生成物 1

HCID 69934936HCID 69934936、化合物収率 100%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

62.8 g (200 milimole) of 2,4-dinitrophenyl cinnamate, 15 g of carbon black with 5% Pt and 2% iron (product with water content of about 50%), and 500 ml of 1,4-dioxane were placed in a reaction vessel (hydrogenating apparatus), and then the reaction mixtures were heated at 60° C. with stirring under a hydrogen atmosphere. In approximately 20 hours, 14.50 L of hydrogen was absorbed, and the reaction was completed when the absorption of hydrogen stopped. Then the reacted solution was separated by filtration to remove the catalyst. The filtrate was concentrated, and 50.8 g of 2,4-diaminophenyl cinnamate was yielded. The exothermic peak temperature was 230° C.

後処理

  1. custom(hydrogenating apparatus), and then the reaction mixtures
  2. custom14.50 L of hydrogen was absorbed
  3. customthe absorption of hydrogen
  4. customThen the reacted solution was separated by filtration
  5. customto remove the catalyst
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-19484faba6d941299f4eb181130fbcfd
出典データセット
uspto-grants-2001_10
特許番号
US06303742B1

反応ノート

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