Acetonitrile → 4-(Trifluoromethoxy)benzoyl azide

HRID 1388366

反応式

HRID 1388366 の反応式
[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8](F)=[O:9])=[CH:6][CH:5]=1.[N-:15]=[N+:16]=[N-:17].[Na+].C1OCCOCCOCCOCCOCCOC1.C(#N)C>C(OCC)C>[F:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([N:15]=[N+:16]=[N-:17])=[O:9])=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 2855718-Crown-6HCID 33557Sodium AzideHCID 67612Benzoyl fluoride, 4-(trifluoromethoxy)-

生成物 1

HCID 132813144-(Trifluoromethoxy)benzoyl azide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 5 grams (24 mmol) of 4-(trifluoromethoxy)benzoyl fluoride, 1.87 grams (29 mmol) of sodium azide, 0.2 grams of 18-Crown-6 ether, and 20 ml. of acetonitrile was stirred at room temperature for two hours under an atmosphere of dry nitrogen. The reaction mixture was diluted with diethyl ether, filtered and concentrated under reduced pressure, with a bath temperature of 40° C., to give the title compound as a turbid oil. IR showed adsorptions at 2280, 2240 and 1695 cm-1.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated under reduced pressure, with a bath temperature of 40° C.

出典と根拠

ORDレコード
ord-f79fc335e7344fa0a0035b33648b6dbd
出典データセット
uspto-grants-1984_02
特許番号
US04431667

関連ノート

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