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

HRID 574143ノート

反応式

HRID 574143 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

At 50° C., 3.1 g (17.55 mmol) of 5-chlorothiophene-2-carbohydrazide were finely suspended in 30 ml of dry THF. 1.81 g (17.90 mmol) of 1-isocyanato-2-methoxyethane dissolved in 30 ml of THF were then 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 diethyl ether was added to the residue. The crystals were filtered off with suction, washed with diethyl ether and dried under high vacuum. This gave 4.87 g (100% of theory) of the title compound.

後処理

  1. customAt 50° C.
  2. additionwere then added dropwise
  3. temperatureAfter cooling to RT
  4. customthe solvent was removed on a rotary evaporator, and diethyl ether
  5. additionwas added to the residue
  6. filtrationThe crystals were filtered off with suction
  7. washwashed with diethyl ether
  8. customdried under high vacuum

出典と根拠

ORDレコード
ord-e655ef45f5854e96bf4ef89bc139a608
出典データセット
uspto-grants-2015_05
特許番号
US09034855B2

反応ノート

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