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Dichloromethane → N-(2,6-diisopropylphenyl)-2-[1-(4-methanesulfonyl-phenyl)-2,4-dioxo-1,3-diazaspiro[4.5]dec-3-yl]acetamide

HRID 1966960
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HRID 1966960 반응식
O[O:2][S:3]([O-:5])=O.[K+].C([C:9]1[CH:14]=[CH:13][C:12]([N:15]2[C:19]3([CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[C:18](=[O:25])[N:17]([CH2:26][C:27]([NH:29][C:30]3[C:35]([CH:36]([CH3:38])[CH3:37])=[CH:34][CH:33]=[CH:32][C:31]=3[CH:39]([CH3:41])[CH3:40])=[O:28])[C:16]2=[O:42])=[CH:11][CH:10]=1)#N.Cl[CH2:44]Cl>CO.O>[CH:36]([C:35]1[CH:34]=[CH:33][CH:32]=[C:31]([CH:39]([CH3:41])[CH3:40])[C:30]=1[NH:29][C:27](=[O:28])[CH2:26][N:17]1[C:18](=[O:25])[C:19]2([CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[N:15]([C:12]2[CH:11]=[CH:10][C:9]([S:3]([CH3:44])(=[O:5])=[O:2])=[CH:14][CH:13]=2)[C:16]1=[O:42])([CH3:37])[CH3:38]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 23707502Potassium hydroxy sulfiteHCID 468924802-[1-(4-cyanophenyl)-2,4-dioxo-1,3-diaza-spiro[4.5]dec-3-yl]-N-(2,6-diisopropylphenyl)acetamide

생성물 1

HCID 46892483N-(2,6-diisopropylphenyl)-2-[1-(4-methanesulfonyl-phenyl)-2,4-dioxo-1,3-diazaspiro[4.5]dec-3-yl]acetamide

시약·촉매·용매 2

HCID 887Methanol
용매
HCID 962Water용매2회

실험 절차

0.421 g (0.684 mmol; 2.2 eq.) of oxone is added to a solution of 0.158 g (0.311 mmol; 1 eq.) of N-(2,6-diisopropylphenyl)-2-[1-(4-methylsulfanylphenyl)-2,4-dioxo-1,3-diazaspiro[4.5]dec-3-yl]acetamide (prepared according to Example 2) in 5 ml of methanol and 2 ml of demineralized water. The reaction medium is stirred at room temperature for 18 hours. Water and dichloromethane are added, and the organic phase is washed several times with water, dried over sodium sulfate and then concentrated to dryness. The product N-(2,6-diisopropylphenyl)-2-[1-(4-methanesulfonyl-phenyl)-2,4-dioxo-1,3-diazaspiro[4.5]dec-3-yl]acetamide is obtained in the form of a solid.

후처리

  1. washthe organic phase is washed several times with water
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-45627f7dc80c46d09c41cf6f169bad0a
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420682B2

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