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Thionyl Chloride → 5-Bromo-benzo[2,1,3]thiadiazole

HRID 335365
Notes
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Reaction equation

HRID 335365 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[CH:6][CH:7]=1.CCN(C(C)C)C(C)C.O=[S:20](Cl)Cl>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[C:4]([CH:3]=1)=[N:9][S:20][N:8]=2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 24386Thionyl ChlorideHCID 81531DiisopropylethylamineHCID 3235934-Bromobenzene-1,2-diamine

Product 1

HCID 27762955-Bromo-benzo[2,1,3]thiadiazole

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 4-bromobenzene-1,2-diamine (5.236 g, 28.0 mmol) and Hunig's base (19.5 mL, 112 mmol) in dichloromethane (160 mL) was added SOCl2 (4.08 mL, 56 mmol) dropwise at room temperature. The resulting reaction mixture was heated to reflux overnight. The reaction mixture was then allowed to cool to room temperature, and quenched with 10% HCl until pH=2. The resulting mixture was extracted with dichloromethane (200 mL×4), dried over Na2SO4 and concentrated. The crude compound was purified by flash column chromatography (silica gel, chloroform) to afford 5-bromobenzo[1,2,5]thiadiazole as a brown solid which was used directly in the next step. 1H NMR (CDCl3 500 MHz): δ: 8.21 (d, 1H, J=1.5 Hz), 7.87 (d, 1H, J=8.5 Hz), 7.69 (dd, 1H, J=8.5, 1.5 Hz).

Workup

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux overnight
  4. customquenched with 10% HCl until pH=2
  5. extractionThe resulting mixture was extracted with dichloromethane (200 mL×4)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customThe crude compound was purified by flash column chromatography (silica gel, chloroform)

Sources & evidence

ORD record
ord-1a6cb30ffed0483dbedae0a181a47844
Source dataset
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08883958B2

Reaction notes

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