5-Chlorothiophene-2-carboxylic acid hydrazide → 2-[(5-Chloro-2-thienyl)carbonyl]-N-(2-methoxyethyl)hydrazinecarboxamide

HRID 2402819ノート

反応式

HRID 2402819 の反応式
[Cl:1][C:2]1[S:6][C:5]([C:7]([NH:9][NH2:10])=[O:8])=[CH:4][CH:3]=1.[N:11]([CH2:14][CH2:15][O:16][CH3:17])=[C:12]=[O:13]>C1COCC1>[Cl:1][C:2]1[S:6][C:5]([C:7]([NH:9][NH:10][C:12]([NH:11][CH2:14][CH2:15][O:16][CH3:17])=[O:13])=[O:8])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 27579235-Chlorothiophene-2-carboxylic acid hydrazideHCID 144050071-Isocyanato-2-methoxyethane

生成物 1

HCID 595369432-[(5-Chloro-2-thienyl)carbonyl]-N-(2-methoxyethyl)hydrazinecarboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

A quantity of 3.1 g (17.55 mmol) of 5-chlorothiophene-2-carbohydrazide was suspended largely finely in 30 ml of dry THF at 50° C. Then 1.81 g (17.90 mmol) of 1-isocyanato-2-methoxyethane in solution in 30 ml of THF were added dropwise. The mixture was stirred at 50° C. for 2.5 h. After cooling to RT, the solvent was removed on a rotary evaporator and the residue was admixed with diethyl ether. The crystals were filtered off with suction, washed with diethyl ether and dried in an HV. This gave 4.87 g (100% of theory) of the title compound.

後処理

  1. temperatureAfter cooling to RT
  2. customthe solvent was removed on a rotary evaporator
  3. filtrationThe crystals were filtered off with suction
  4. washwashed with diethyl ether
  5. customdried in an HV

出典と根拠

ORDレコード
ord-282fc92243b74bc0a0a8ac62eec55c8d
出典データセット
uspto-grants-2014_08
特許番号
US08796324B2

反応ノート

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