Sodium hydride → HCID 21525530, compound

HRID 1658794Notes

Reaction equation

HRID 1658794 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]([N:11]2[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=3[N:15]3[C:22](=[O:25])[NH:23][N:24]=[C:14]3[C:13]3[CH:26]=[CH:27][CH:28]=[N:29][C:12]2=3)=[O:10])[CH2:4][CH2:3]1.[H-].[Na+].[N:32]1([CH2:37][CH2:38][CH2:39]Cl)[CH2:36][CH2:35][CH2:34][CH2:33]1>CN(C)C=O.C1(C)C(C)=CC=CC=1>[N:32]1([CH2:37][CH2:38][CH2:39][N:23]2[C:22](=[O:25])[N:15]3[C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=4[N:11]([C:9](=[O:10])[CH2:8][N:5]4[CH2:4][CH2:3][N:2]([CH3:1])[CH2:7][CH2:6]4)[C:12]4[N:29]=[CH:28][CH:27]=[CH:26][C:13]=4[C:14]3=[N:24]2)[CH2:36][CH2:35][CH2:34][CH2:33]1

Participants

6

Reactant 3

HCID 24758Sodium hydrideHCID 113210281-(3-Chloropropyl)-pyrrolidineHCID 21525592HCID 21525592, compound

Product 1

HCID 21525530HCID 21525530, compound

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 7237O-XyleneSolvent

Procedure

In the manner given in Example 25, to 2,9-dihydro-9-[(4-methylpiperazino)acetyl]-3H-pyrido[3,2-c]-s-triazolo[4,3-a][1,5]benzodiazepin-3-one in dimethylformamide is added a solution of sodium hydride in mineral oil. The mixture is allowed to react at about 95° C. for 40 minutes and after cooling (3-pyrrolidinopropyl)chloride in xylene is added. The mixture is kept at 95°-100°C. for a period of 22 hours, evaporated and worked up as in example 25 to give 2,9-dihydro-2-(3-pyrrolidinopropyl)-9-[(4-methylpiperazino)acetyl]-3H-pyrido[3,2-c]-s-triazolo[4,3-a][1,5]benzodiazepin-3-one.

Workup

  1. customto react at about 95° C. for 40 minutes
  2. additionis added
  3. customevaporated

Sources & evidence

ORD record
ord-cf05cb37b2a04675b4bbd7fc585f2544
Source dataset
uspto-grants-1976_06
Patent number
US03966736

Reaction notes

Loading…