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Dimethyl Sulfoxide → HCID 53765127, 화합물

HRID 1706852
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HRID 1706852 반응식
I[C:2]([F:11])([F:10])[C:3]([F:9])([F:8])[C:4]([F:7])([F:6])I.I[C:13]1[CH:14]=[C:15]([C:21]#[N:22])[C:16](=[CH:19][CH:20]=1)[C:17]#[N:18].CS(C)=O>[Cu].O>[C:21]([C:15]1[CH:14]=[C:13]([C:2]([F:11])([F:10])[C:3]([F:9])([F:8])[C:4]([F:7])([F:6])[C:13]2[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[C:15]([C:21]#[N:22])[CH:14]=2)[CH:20]=[CH:19][C:16]=1[C:17]#[N:18])#[N:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 679Dimethyl SulfoxideHCID 41200244-IodophthalonitrileHCID 109164621,1,2,2,3,3-Hexafluoro-1,3-diiodopropane

생성물 1

HCID 53765127HCID 53765127, 화합물수율 54.4%

시약·촉매·용매 2

HCID 23978Copper촉매HCID 962Water용매

실험 절차

1,3-Diiodoperfluoropropane (2.0 g, 5 mmol), 1.8 g (30 meq) of activated copper, 2.5 g (10 mmol) of 4-iodophthalonitrile and 6 ml of dry dimethyl sulfoxide were purged for 15 minutes with argon and the mixture was then heated at 115°-120° C. for 4 hours. After cooling, the content was poured into 100 ml of water and extracted with four 50 ml portions of ether. The combined ethereal extract was washed with water, charcoaled, dried over anhydrous sodium sulfate and concentrated at reduced pressure to afford 1.1 g (52%) of product, m.p 133°-135° C.

후처리

  1. temperaturethe mixture was then heated at 115°-120° C. for 4 hours
  2. temperatureAfter cooling
  3. extractionextracted with four 50 ml portions of ether
  4. extractionThe combined ethereal extract
  5. washwas washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated at reduced pressure

출처 및 근거

ORD 기록
ord-b9b6eba7bfc346d2ac3d9b4e5c110e2d
출처 데이터셋
uspto-grants-1980_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04209458

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