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1,3-Dipropyl-2-thiourea → 2-[(Propylamino)(propylimino)methylthio]-3-quinoxalinecarboxylic acid ethyl ester, hydrochloride

HRID 1702846
ノート
印刷プレビュー

反応式

HRID 1702846 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].[CH2:17]([NH:20][C:21]([NH:23][CH2:24][CH2:25][CH3:26])=[S:22])[CH2:18][CH3:19]>CC(C)=O>[ClH:16].[CH2:1]([O:3][C:4]([C:6]1[C:7]([S:22][C:21]([NH:23][CH2:24][CH2:25][CH3:26])=[N:20][CH2:17][CH2:18][CH3:19])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 28012141,3-Dipropyl-2-thioureaHCID 12283436Ethyl 3-Chloroquinoxaline-2-carboxylate

生成物 1

HCID 1317128382-[(Propylamino)(propylimino)methylthio]-3-quinoxalinecarboxylic acid ethyl ester, hydrochloride

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (3.551 g., 0.015 mole) and 2.405 g. (0.015 mole) of 1,3-di-n-propylthiourea were dissolved in acetone and heated at reflux for 11/2 hours. The solution was concentrated to a volume of 50 ml. and cooled. A small amount of solid was removed by filtration. The filtrate was further concentrated to a volume of 25 ml. and ether was added to turbidity. After the reaction mixture had been cooled the yellow solid was collected by filtration to give 2.77 g. (46.6%) of the product, m.p. 129°-130° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 11/2 hours
  3. concentrationThe solution was concentrated to a volume of 50 ml
  4. temperatureand cooled
  5. customA small amount of solid was removed by filtration
  6. concentrationThe filtrate was further concentrated to a volume of 25 ml
  7. additionand ether was added to turbidity
  8. temperatureAfter the reaction mixture had been cooled the yellow solid
  9. filtrationwas collected by filtration
  10. customto give 2.77 g

出典と根拠

ORDレコード
ord-fa6568838bfc4132b2fd45d569acd97c
出典データセット
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04349674

反応ノート

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