Aluminium lithium hydride → HCID 59703212, compound

HRID 1365599Notes

Reaction equation

HRID 1365599 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]1[S:9][C:10]2[C:16]3[N:17]([C:26]4[CH:36]=[CH:35][C:29]([C:30]([N:32]([CH3:34])[CH3:33])=O)=[CH:28][C:27]=4[Cl:37])[N:18]=[C:19]([C:20]4[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=4)[C:15]=3[CH2:14][CH2:13][C:11]=2[N:12]=1>C1COCC1>[Cl:37][C:27]1[CH:28]=[C:29]([CH2:30][N:32]([CH3:34])[CH3:33])[CH:35]=[CH:36][C:26]=1[N:17]1[C:16]2[C:10]3[S:9][C:8]([NH2:7])=[N:12][C:11]=3[CH2:13][CH2:14][C:15]=2[C:19]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)=[N:18]1

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 59255573HCID 59255573, compound

Product 1

HCID 59703212HCID 59703212, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Under an argon atmosphere at −78° C. a solution of lithium aluminium hydride (1 M in THF, 3 mL) is added to a solution of 4-(7-amino-3-pyridin-3-yl-4,5-dihydro-pyrazolo[4,3-g]benzothiazol-1-yl)-3-chloro-N,N-dimethylbenzamide (PCT/EP05055021) (0.46 g, 1 mmol) in 25 mL dry THF. After 5 min the cooling bath is removed and the reaction mixture is heated to RT. Then while cooling, 1 mL of water is added dropwise and the mixture is stirred for 30 min. The precipitate is filtered and the filtrate evaporated down.

Workup

  1. customAfter 5 min the cooling bath is removed
  2. temperatureThen while cooling
  3. addition1 mL of water is added dropwise
  4. filtrationThe precipitate is filtered
  5. customthe filtrate evaporated down

Sources & evidence

ORD record
ord-5827990c6c2947bcb85757efcdbe76b7
Source dataset
uspto-grants-2011_02
Patent number
US07893049B2

Reaction notes

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