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Hydrochloric Acid → HCID 178420508, compound

HRID 1919679
Notes
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Reaction equation

HRID 1919679 reaction equation
[N-:1]=[N+:2]=[N-:3].[Na+].[Al](Cl)(CC)CC.[O:11]([C:18]1[C:27]2[CH:28]=[CH:29][S:30][C:26]=2[C:25]2[CH:24]=[CH:23][C:22]([C:31]#[N:32])=[CH:21][C:20]=2[N:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Al](N=[N+]=[N-])(CC)CC.[OH-].[Na+].N([O-])=O.[Na+].Cl>>[O:11]([C:18]1[C:27]2[CH:28]=[CH:29][S:30][C:26]=2[C:25]2[CH:24]=[CH:23][C:22]([C:31]3[NH:32][N:3]=[N:2][N:1]=3)=[CH:21][C:20]=2[N:19]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 7

HCID 313Hydrochloric AcidHCID 7277Diethylaluminum chlorideHCID 14798Sodium HydroxideHCID 33557Sodium AzideHCID 166873163-(Diethylalumanyl)triaza-1,2-dien-2-ium-1-ideHCID 23668193Sodium NitriteHCID 57500695
HCID 57500695, compound

Product 1

HCID 178420508HCID 178420508, compound

Procedure

In an oven dried flask, under nitrogen atmosphere, was charged sodium azide (1.4 eq, 84 mg). Et2AlCl (1.4 eq, 1.08 ml of 1.8 M solution in toluene) was added through syringe. The mixture was stirred at room temperature for 4 hours. 4-phenoxythieno[3,2-c]quinoline-7-carbonitrile (1.0 eq, 20 mg) was charged in a vial. Et2AlN3 solution (0.15 ml) was added and the resulting mixture stirred at 80° C. for 5 days. The mixture was treated by a solution of NaOH and some sodium nitrite was added (pH=13-14). The pH was adjusted to 1.5 with HCl 6N. The material was extracted with ethyl acetate. The material was extracted from the organic phase using a saturated aqueous solution of K2CO3. The pH was adjusted to 2.5 with HCl 6N and the material was extracted with ethyl acetate. The solvent were evaporated to afford 4-phenoxy-7-(1H-tetrazol-5-yl)thieno[3,2-c]quinoline. LCMS (ES)>95% pure, m/z 303 [M+1]+.

Workup

  1. customIn an oven dried flask
  2. stirringthe resulting mixture stirred at 80° C. for 5 days
  3. extractionThe material was extracted with ethyl acetate
  4. extractionThe material was extracted from the organic phase
  5. extractionthe material was extracted with ethyl acetate
  6. customThe solvent were evaporated

Sources & evidence

ORD record
ord-1204382e35014fb7b0336f0aed4e85bc
Source dataset
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08168651B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes