Ethylene Glycol → 7-Chloro-2-(2-hydroxyethoxy)-5-phenyl-3H-1,4-benzodiazepine

HRID 649267

反応式

HRID 649267 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12]P(N3CCOCC3)(N3CCOCC3)=O)[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1.C(N(CC)CC)C.[CH2:41](O)[CH2:42][OH:43]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12][CH2:41][CH2:42][OH:43])[CH2:9][N:8]=[C:7]([C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)[C:6]=2[CH:33]=1

参加物

4

反応物 3

HCID 174Ethylene GlycolHCID 8471TriethylamineHCID 149078867-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin

生成物 1

HCID 122845957-Chloro-2-(2-hydroxyethoxy)-5-phenyl-3H-1,4-benzodiazepine

実験手順

A suspension of 1.95 g (4.0 mmoles) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin in 10 ml of ethylene glycol containing 4 ml of triethylamine was heated on a steam bath for 2 hrs. A clear solution formed soon after heating began. Triethylamine was removed in vacuo. The ethylene glycol solution was poured into ice water precipitating solids which were collected and washed thoroughly with water. Remaining water was removed from the solid by dissolving in solid in ether, drying over sodium sulfate and evaporation of ether. Crystallization of the residue from ether-hexane gave colorless prisms, mp 142°-144°.

後処理

  1. temperaturewas heated on a steam bath for 2 hrs
  2. customA clear solution formed soon
  3. temperatureafter heating
  4. customTriethylamine was removed in vacuo
  5. additionThe ethylene glycol solution was poured into ice water precipitating solids which
  6. customwere collected
  7. washwashed thoroughly with water
  8. customRemaining water was removed from the solid
  9. dissolutionby dissolving in solid in ether
  10. dry with materialdrying over sodium sulfate and evaporation of ether
  11. customCrystallization of the residue from ether-hexane
  12. customgave colorless prisms, mp 142°-144°

出典と根拠

ORDレコード
ord-8d84581afc1947669a234219566ec716
出典データセット
uspto-grants-1988_04
特許番号
US04739049

関連ノート

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