Diethyl Ether → 2-[(3-chloro-4-methyl-2-thienyl)carbonyl]-N-isobutylhydrazinecarboxamide

HRID 660912

반응식

HRID 660912 반응식
[Cl:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([NH:10][NH2:11])=[O:9].[CH2:12]([N:16]=[C:17]=[O:18])[CH:13]([CH3:15])[CH3:14].C(OCC)C>C1COCC1>[Cl:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([NH:10][NH:11][C:17]([NH:16][CH2:12][CH:13]([CH3:15])[CH3:14])=[O:18])=[O:9]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 612812-Methylpropyl isocyanateHCID 27775683-Chloro-4-methyl-2-thiophenecarboxylic acid hydrazide

생성물 1

HCID 580122082-[(3-chloro-4-methyl-2-thienyl)carbonyl]-N-isobutylhydrazinecarboxamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

1.00 g (5.25 mmol) of 3-chloro-4-methylthien-2-ylcarboxylic acid hydrazide are placed in 10 ml THF at room temperature. 520 mg (5.25 mmol) of isobutyl isocyanate, dissolved in 2 ml THF, are rapidly added dropwise with stirring. The mixture is further stirred overnight at room temperature. For the workup, the reaction mixture is treated with 10 ml diethyl ether, cooled in the water/ice-bath to about 0° C., and the resulting precipitate recovered by filtration, washed with diethyl ether and dried in vacuo. 1.29 g (85% of theory) of the target compound are thus obtained.

후처리

  1. additionare rapidly added dropwise
  2. filtrationthe resulting precipitate recovered by filtration
  3. washwashed with diethyl ether
  4. customdried in vacuo
  5. custom1.29 g (85% of theory) of the target compound are thus obtained

출처 및 근거

ORD 기록
ord-b86eac4de23e4e6ea08a2140093682a2
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084481B2

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