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Methanol → 1-Methyl-4-[(1,3,4,4-tetrachloro-2-nitrobuta-1,3-dien-1-yl)sulfanyl]benzene

HRID 2055666
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HRID 2055666 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[N+:9]([C:12]([C:16]([Cl:20])=[C:17]([Cl:19])[Cl:18])=[C:13](Cl)[Cl:14])([O-:11])=[O:10].CO>CCOCC>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:13]([Cl:14])=[C:12]([N+:9]([O-:11])=[O:10])[C:16]([Cl:20])=[C:17]([Cl:18])[Cl:19])=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 887MethanolHCID 78114-MethylbenzenethiolHCID 379884NSC665076

생성물 1

HCID 713532881-Methyl-4-[(1,3,4,4-tetrachloro-2-nitrobuta-1,3-dien-1-yl)sulfanyl]benzene

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

At room temperature, 4.72 g (38 mmol) of 4-methylthiophenol are added to a solution of 10.00 g (36.9 mmol) of 2-nitropentachloro-1,3-butadiene in 20 ml of ether, and the mixture is stirred for 20 h. The ether is then removed under reduced pressure, and the crystal slurry which is formed after addition of 20 ml of methanol is filtered off, washed with cold MeOH (2×10 ml) and dried under reduced pressure, yield 9.9 g (75%), Rf=0.72 (Et2O: petroleum ether=1:3), m.p. 110-111° C.

후처리

  1. customThe ether is then removed under reduced pressure
  2. customthe crystal slurry which is formed
  3. filtrationis filtered off
  4. washwashed with cold MeOH (2×10 ml)
  5. dry with materialdried under reduced pressure, yield 9.9 g (75%), Rf=0.72 (Et2O: petroleum ether=1:3), m.p. 110-111° C.

출처 및 근거

ORD 기록
ord-eec9090e7b68484287415fe05c8b73b3
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07332512B2

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