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

HRID 574143노트

반응식

HRID 574143 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e655ef45f5854e96bf4ef89bc139a608
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034855B2

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