Sodium Azide → 4-(Azidomethyl)-2,2-bis(trifluoromethyl)-1,3-dioxolane

HRID 1439524ノート

反応式

HRID 1439524 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1([C:20]([F:23])([F:22])[F:21])[O:7][CH:6]([CH2:8]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:5][O:4]1.[N-:26]=[N+:27]=[N-:28].[Na+]>CN(C)C=O.C1C=CC=CC=1>[F:1][C:2]([F:25])([F:24])[C:3]1([C:20]([F:23])([F:22])[F:21])[O:7][CH:6]([CH2:8][N:26]=[N+:27]=[N-:28])[CH2:5][O:4]1

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 21395816HCID 21395816、化合物

生成物 1

HCID 213958034-(Azidomethyl)-2,2-bis(trifluoromethyl)-1,3-dioxolane

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 6228Dimethylformamide溶媒

実験手順

A sample of 14.00 grams of 2,2-bis(trifluoromethyl)-4-tosyloxymethyl-1,3-dioxolane (m.p. 58°-60° C.) is dissolved in 40 ml of dimethylformamide and 4.85 grams NaN3 is added. The mixture is stirred magnetically at 140°-149° C. for 3.5 hours. The product is diluted with benzene and filtered. The filtrate is washed thoroughly with water, vacuum-stripped and distilled. The product, 2,2-bis(trifluoromethyl)-4-azidomethyl-1,3-dioxolane, has a boiling point of 78° C./20 mm Hg and a refractive index of 1.37447 at 20° C. Analysis Found: (In Percent) C, 26.95; H, 1.73; N, 16.06. Calculated for C6H5F6N3O2 (M.W. 265.1): C, 27.18; H, 1.90; N, 15.84.

後処理

  1. filtrationfiltered
  2. washThe filtrate is washed thoroughly with water
  3. distillationvacuum-stripped and distilled
  4. customat 20° C

出典と根拠

ORDレコード
ord-5c566e98631c4829a51ab641ae970fde
出典データセット
uspto-grants-1977_11
特許番号
US04060532

反応ノート

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