Methane → Carbamic fluoride, diphenyl-

HRID 364877

反応式

HRID 364877 の反応式
[C:1]1([N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8](Cl)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Sb](F)(F)[F:19].C>C1(C)C(C)=CC=CC=1.CO>[C:1]1([N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([F:19])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

7

反応物 4

HCID 297MethaneHCID 312ChlorideHCID 24554Antimony trifluorideHCID 65741N,N-Diphenylcarbamic chloride

生成物 1

HCID 20238555Carbamic fluoride, diphenyl-

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 7237O-Xylene溶媒

実験手順

DPFC was prepared according to a published method of Metzger and Wilson (Biochem., 1964, Vol. 3, pp 926-931). Diphenylcarbamyl Chloride was obtained from Aldrich Chemical Co. Inc., Milwaukee, Wis., USA. DFPC was prepared from the chloride by reaction with 50% excess antimony trifluoride in hot xylene for one hour. The mixture was cooled to room temperature. Antimony halides were then precipitated with ether and the solution decolorized with charcoal, filtered and evaporated to dryness. The solids thus obtained were dissolved in Methanol, decolorized with charcoal, filtered and crystalized by cooling the solution to about 0° C. This process was repeated again and yielded white crystals with melting point of 81°-82° C.

後処理

  1. customDPFC was prepared
  2. customAntimony halides were then precipitated with ether
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe solids thus obtained
  6. filtrationfiltered
  7. customcrystalized
  8. temperatureby cooling the solution to about 0° C
  9. customyielded white crystals with melting point of 81°-82° C.

出典と根拠

ORDレコード
ord-5c8d4e64302f449092807a9e54ddb043
出典データセット
uspto-grants-1986_08
特許番号
US04607010

関連ノート

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