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Dimethyl Sulfoxide → HCID 53765127、化合物

HRID 1447055
ノート
印刷プレビュー

反応式

HRID 1447055 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 53765127HCID 53765127、化合物収率 54.4%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c5e1d09fa4174fab821dc4f77c7d3628
出典データセット
uspto-grants-1982_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04315093

反応ノート

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