Methyl iodide → 1H-1,4-Benzodiazepine

HRID 441398

반응식

HRID 441398 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:11]3C(CON)=NN=[C:10]3[CH2:9][N:8]=[C:7](C3C=CC=CC=3)[C:6]=2[CH:24]=1.[H-].[Na+].CI>CN(C)C=O>[NH:11]1[C:5]2[CH:4]=[CH:3][CH:2]=[CH:24][C:6]=2[CH:7]=[N:8][CH:9]=[CH:10]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 126124268-chloro-1-[(aminooxy)methyl]6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine

생성물 1

HCID 1484311H-1,4-Benzodiazepine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred solution of 8-chloro-1-[(aminooxy)methyl]6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine (0.02 mole) in dry dimethylformamide (50 ml.) is cooled in an ice bath under nitrogen and treated successively with a 57% mineral oil suspension of sodium hydride (0.84 g,. 0.02 mole) and methyliodide (0.02 mole). The mixture is allowed to come slowly to ambient temperature and stand for 18 hours. It is then concentrated in vacuo. The residue is chromatographed on silica gel with methanol to give 8-chloro-1-[[(methylamino)oxy]methyl]6-phenyl-4H-s-triazolo]4,3-a][1,4]benzodiazepine.

후처리

  1. customto come slowly to ambient temperature
  2. concentrationIt is then concentrated in vacuo
  3. customThe residue is chromatographed on silica gel with methanol

출처 및 근거

ORD 기록
ord-d01ab87d9aa44073b1d7ec8d3cec7ccd
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04039551

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