Methane → HCID 131712839、化合物

HRID 1702847

反応式

HRID 1702847 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7]([Cl:16])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2].C.[CH2:18]([NH:22][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[S:24])[CH2:19][CH2:20][CH3:21]>CC(C)=O>[ClH:16].[CH2:1]([O:3][C:4]([C:6]1[C:7]([S:24][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[N:22][CH2:18][CH2:19][CH2:20][CH3:21])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 297Methane2 回HCID 2723622N,N'-DibutylthioureaHCID 12283436Ethyl 3-Chloroquinoxaline-2-carboxylate

生成物 1

HCID 131712839HCID 131712839、化合物収率 47.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (7.10 g., 0.03 mole) was dissolved in 125 ml. of acetone treated with Norit and filtered. The filtrate was added to 5.650 g. (0.03 mole) of 1,3-di-n-butylthiourea in 100 ml. of acetone. The solution was stirred at reflux under a nitrogen atmosphere for 6 hours, allowed to cool to room temperature, and stirred an additional 17 hours. The red solution was treated with Norit, filtered, and concentrated to a volume of 100 ml. The yellow solid that crystallized out was collected by filtration, washed and dried to give the 6.05 g. (47.5% yield) of product, m.p. 138°-139° C. (dec.).

後処理

  1. filtrationfiltered
  2. additionThe filtrate was added to 5.650 g
  3. temperatureat reflux under a nitrogen atmosphere for 6 hours
  4. stirringstirred an additional 17 hours
  5. filtrationfiltered
  6. concentrationconcentrated to a volume of 100 ml
  7. customThe yellow solid that crystallized out
  8. filtrationwas collected by filtration
  9. washwashed
  10. customdried
  11. customto give the 6.05 g

出典と根拠

ORDレコード
ord-f825206e528846759b677540039b12f1
出典データセット
uspto-grants-1982_09
特許番号
US04349674

関連ノート

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