Tetrahydrofuran → 1-[2-(1,3,5-Triethylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine

HRID 579247노트

반응식

HRID 579247 반응식
[CH3:1][NH:2][N:3]=[C:4]([CH3:10])[CH2:5][S:6]([CH3:9])(=[O:8])=[O:7].O1CCCC1.C(N(CC)CC)C.[CH2:23]([C:25]1([C:35](=[O:39])[C:36](Cl)=[O:37])[CH:30]=[C:29]([CH2:31][CH3:32])[CH:28]=[C:27]([CH2:33][CH3:34])[CH2:26]1)[CH3:24]>CCCCCC>[CH2:23]([C:25]1([C:35](=[O:39])[C:36]([N:2]([CH3:1])[N:3]=[C:4]([CH3:10])[CH2:5][S:6]([CH3:9])(=[O:8])=[O:7])=[O:37])[CH:30]=[C:29]([CH2:31][CH3:32])[CH:28]=[C:27]([CH2:33][CH3:34])[CH2:26]1)[CH3:24]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 764689591-Methyl-2-(1-methylsulfonyl-2-propylidene)hydrazineHCID 866893512-(1,3,5-Triethylphenyl)-2-oxoacetyl chloride

생성물 1

HCID 866893521-[2-(1,3,5-Triethylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine수율 75%

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
0 °C

실험 절차

To a 3 L volume four-necked flask, 1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine (5-2-1) (116.0 g), tetrahydrofuran (anhydrous) (600 ml), and triethylamine (98.5 ml) were added under a nitrogen atmosphere, and cooled to about 1° C. to the mixture, 2-(1,3,5-triethylphenyl)-2-oxoacetyl chloride (6-b) (178.5 g) was added dropwise, and stirred at 0° C. for 1 hour. The reaction mixture was added dropwise to hexane (3 L) at room temperature, and stirred for 1 hour. The precipitated solids were collected by filtration, washed with hexane (0.5 L×2) and water (0.5 L×6), and dried under reduced pressure to give 200.9 g of 1-[2-(1,3,5-triethylphenyl)-2-oxoacetyl]-1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine ((4-34)-(1)-40).

후처리

  1. additionwas added dropwise
  2. stirringstirred for 1 hour
  3. filtrationThe precipitated solids were collected by filtration
  4. washwashed with hexane (0.5 L×2) and water (0.5 L×6)
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-43e4446a82624c0db6641edec0cbda45
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040709B2

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