Methyl pyruvate → HCID 53751159、化合物

HRID 328381

反応式

HRID 328381 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10](NN)[CH2:9][N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.C(OC)(=O)C(C)=O>CO>[C:14]1([C:7]2[C:6]3[CH:20]=[CH:2][CH:3]=[CH:4][C:5]=3[N:11]=[CH:10][CH2:9][N:8]=2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 11748Methyl pyruvate2 回HCID 123908747-Chloro-2-hydrazinyl-5-phenyl-3H-1,4-benzodiazepine

生成物 1

HCID 53751159HCID 53751159、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 5.7 g. (0.02 mole) of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine, 3 ml. (0.04 mole) of methyl pyruvate and 50 ml. of methanol is stirred, under nitrogen, for 17 hours at room temperature, by which time the solid has dissolved. Three ml. more methyl pyruvate is added and the solution is allowed to stand for 7 hours more. After filtration and evaporation in vacuo (50° C./0.5 mm.) a brown gum is obtained which is chromatographed on silica gel and eluted with 1% methanol in chloroform. Evaporation of the combined fractions containing the product (as indicated by thin layer chromatography) gives a gum which is crystallized from a mixture of chloroform and ether. A yield of 3.5 g. (67%) of 7-chloro-2-[[1-methoxycarbonyl)ethylidene]hydrazino]-5-phenyl-3H-1,4-benzodiazepine is obtained as nearly white crystals of melting point 156°-157° C. Melt solvate indicates the product contained 1.95% CHCl3 even after prolonged drying in vacuo.

後処理

  1. additionA mixture of 5.7 g
  2. dissolutionhas dissolved
  3. filtrationAfter filtration and evaporation in vacuo (50° C./0.5 mm.) a brown gum
  4. customis obtained which
  5. customis chromatographed on silica gel
  6. washeluted with 1% methanol in chloroform
  7. customEvaporation of the combined fractions
  8. additioncontaining the product (as indicated by thin layer chromatography)
  9. customgives a gum which
  10. customis crystallized from a mixture of chloroform and ether

出典と根拠

ORDレコード
ord-e62459c7d01d41e2bcecb80f4214d39b
出典データセット
uspto-grants-1977_04
特許番号
US04017492

関連ノート

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