Water → HCID 12837764, compound

HRID 1902195Notes

Reaction equation

HRID 1902195 reaction equation
[C:1]([CH2:5][N:6]1[CH2:23][CH2:22][N:9]2[C:10]3[CH:21]=[CH:20][CH:19]=[CH:18][C:11]=3[CH2:12][N:13]3[CH:17]=[CH:16][CH:15]=[C:14]3[CH:8]2[CH2:7]1)(OC)=[O:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[OH:2][CH2:1][CH2:5][N:6]1[CH2:23][CH2:22][N:9]2[C:10]3[CH:21]=[CH:20][CH:19]=[CH:18][C:11]=3[CH2:12][N:13]3[CH:17]=[CH:16][CH:15]=[C:14]3[CH:8]2[CH2:7]1

Participants

6

Reactant 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 13103372HCID 13103372, compoundHCID 21226445Aluminium lithium hydride

Product 1

HCID 12837764HCID 12837764, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To the solution of 780 mg of 2-carbomethoxymethyl-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]-benzodiazepine in 20 ml of tetrahydrofuran, 150 mg of lithium aluminum hydride are added and the mixture is stirred for 2 days at room temperature. It is combined with 0.15 ml of water, 0.15 ml of 15% aqueous sodium hydroxide and 0.15 ml of water in this order filtered and the filtrate evaporated, to yield the 2-(2-hydroxyethyl)-1,3,4,14b-tetrahydro-10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]benzodiazepine, which is converted into its mono-fumarate melting at 187°-189° with decomposition.

Workup

  1. filtrationfiltered
  2. customthe filtrate evaporated

Sources & evidence

ORD record
ord-637607e887e44ebdba97974b3457315d
Source dataset
uspto-grants-1982_12
Patent number
US04362666

Reaction notes

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