ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dichloromethane → 7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylic acid isopropyl ester

HRID 1679049
ノート
印刷プレビュー

反応式

HRID 1679049 の反応式
C[O-].[Na+].Cl.[CH:5](OC(C1N(CCN(CC)CC)C(C2C=CC=CC=2)=C2C=1C=CC(Cl)=C2)=O)(C)C.C(Cl)Cl.[CH2:37]([O:39][C:40]([CH:42]1[N:48]=[C:47]([C:49]2[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=2)[C:46]2[CH:55]=[C:56]([Cl:59])[CH:57]=[CH:58][C:45]=2[NH:44][C:43]1=[O:60])=[O:41])[CH3:38]>C(O)(=O)C>[CH:37]([O:39][C:40]([CH:42]1[N:48]=[C:47]([C:49]2[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=2)[C:46]2[CH:55]=[C:56]([Cl:59])[CH:57]=[CH:58][C:45]=2[NH:44][C:43]1=[O:60])=[O:41])([CH3:5])[CH3:38]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 110682Ethyl 7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylateHCID 10942334Sodium MethoxideHCID 706209895-Chloro-2-[2-(diethylamino)ethyl]-3-phenylisoindole-1-carboxylic acid isopropyl ester hydrochloride

生成物 1

HCID 539649407-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylic acid isopropyl ester

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
25 °C

実験手順

500 Ml. of propanol-(2) are treated with 14 g. of sodium methylate; the methanol formed is removed by concentration in vacuo to half the volume and the suspension obtained is diluted with 250 ml. of methylene chloride. Then, 34.2 g. of 7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylic acid ethyl ester are added and the mixture is subsequently stirred at 25° C. for 40 minutes. The orange solution is made acidic with glacial acetic acid and evaporated to dryness under reduced pressure. The residue is partitioned between water and chloroform; the organic phase is washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate and concentrated to dryness. The solid crude product is triturated with ether, removed by filtration, washed with ether and recrystallized from methylene chloride/ether, whereby there is obtained 7-chloro-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine-3-carboxylic acid isopropyl ester having a melting point of 234°-238° C. (decomposition).

後処理

  1. customis removed by concentration in vacuo to half the volume
  2. customthe suspension obtained
  3. additionis diluted with 250 ml
  4. customevaporated to dryness under reduced pressure
  5. customThe residue is partitioned between water and chloroform
  6. washthe organic phase is washed with a saturated aqueous solution of sodium chloride
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated to dryness
  9. customThe solid crude product is triturated with ether
  10. customremoved by filtration
  11. washwashed with ether
  12. customrecrystallized from methylene chloride/ether

出典と根拠

ORDレコード
ord-af8d9f629f914c4181715a3c284ad0ae
出典データセット
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04077978

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート