Aluminium lithium hydride → HCID 68520330, compound

HRID 1811700Notes

Reaction equation

HRID 1811700 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH:7]1[C:12]2[S:13][C:14]3[C:18]4[CH:19]=[CH:20][C:21]([C:23]([O-:25])=[O:24])=[CH:22][C:17]=4[S:16][C:15]=3[C:11]=2[CH:10]=[CH:9][C:8]=1[C:26]([O-:28])=[O:27]>C1COCC1>[OH:28][CH:26]([OH:27])[C:8]1[CH:9]=[CH:10][C:11]2[C:15]3[S:16][C:17]4[CH:22]=[C:21]([CH:23]([OH:24])[OH:25])[CH:20]=[CH:19][C:18]=4[C:14]=3[S:13][C:12]=2[CH:7]=1

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 86637838HCID 86637838, compound

Product 1

HCID 68520330HCID 68520330, compoundYield 143.5%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

LiAlH4(0.74 g, 19.5 mmol) was added to [1]benzothieno[3,2-b]benzothiophene 2,7-dicarboxylate (1.50 g 3.9 mmol) in THF (40 mL). The mixture was stirred overnight. Insoluble materials were removed by filtration and washed with hot DMSO. The solution was precipitated in 50 mL of 1 normal (“N”) HCl. The product was collected by filtration to obtain 1.86 g (75%) of pure 2,7-bis(dihydroxymethyl)[1]benzothieno[3,2-b]benzothiophene.

Workup

  1. customInsoluble materials were removed by filtration
  2. washwashed with hot DMSO
  3. customThe solution was precipitated in 50 mL of 1 normal (“N”) HCl
  4. filtrationThe product was collected by filtration

Sources & evidence

ORD record
ord-8c07cc9b9c3e4e55a9471ca784e95295
Source dataset
uspto-grants-2013_01
Patent number
US08362464B2

Reaction notes

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