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Tin tetrachloride → HCID 21109095, 화합물

HRID 1435710
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HRID 1435710 반응식
[C:1]([C:3]1[C:4]([C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([N+:32]([O-:34])=[O:33])[CH:27]=2)=[N:5][C:6]([S:24][CH3:25])=[N:7][C:8]=1[CH2:9][CH2:10][CH:11](C(OCC)=O)[C:12]([O:14][C:15](C)([CH3:17])C)=[O:13])#[N:2].Cl[Sn](Cl)(Cl)Cl>C(Cl)Cl>[NH2:2][C:1]1[C:3]2[C:4]([C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([N+:32]([O-:34])=[O:33])[CH:27]=3)=[N:5][C:6]([S:24][CH3:25])=[N:7][C:8]=2[CH2:9][CH2:10][C:11]=1[C:12]([O:14][CH2:15][CH3:17])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24287Tin tetrachlorideHCID 86614568HCID 86614568, 화합물

생성물 1

HCID 21109095HCID 21109095, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of tert-butyl ethyl {2-[5-cyano-2-methylthio-4-(3-nitro-phenyl)-pyrimidin-6-yl]-ethyl}-malonate (example 27c, 1.40 g) in CH2Cl2 (15 ml) was cooled to 0° C. A solution of SnCl4 (1 M in CH2Cl2, 11.5 ml) was added dropwise, the ice-bath removed and the solution was stirred for an additional 30 min at room temperature. Water (64 ml) and EtOAc (64 ml) were added and the mixture was vigorously stirred until al solids dissolved. The organic phase was washed with water and brine, dried (MgSO4) and concentrated under reduced pressure, giving the title compound as a crude product.

후처리

  1. customthe ice-bath removed
  2. additionWater (64 ml) and EtOAc (64 ml) were added
  3. stirringthe mixture was vigorously stirred until al solids
  4. dissolutiondissolved
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6045732b2ba04ef39bf56092a217d107
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618963B2

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