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Dimethyl Sulfide → 8-Bromo-2-chloro-5,6,11,12-tetrahydro-dibenzo[b,f]azocine-12-ol

HRID 2220200
Notes
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Reaction equation

HRID 2220200 reaction equation
[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[CH2:6][C:7](=[O:18])[C:8]3[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:9]=3[NH:10][C:11](=O)[C:4]=2[CH:3]=1.CSC>C1COCC1>[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[CH2:6][CH:7]([OH:18])[C:8]3[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:9]=3[NH:10][CH2:11][C:4]=2[CH:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 1068Dimethyl SulfideHCID 597723788-Bromo-2-chloro-5h,11h-dibenzo[b,f]azocine-6-12-dione

Product 1

HCID 597724718-Bromo-2-chloro-5,6,11,12-tetrahydro-dibenzo[b,f]azocine-12-olYield 44%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Conditions

Temperature
70 °C

Procedure

To a mixture of 8-Bromo-2-chloro-5H,11H-dibenzo[b,f]azocine-6-12-dione (2.0 g, 5.7 mmole) in THF (20 mL) was added a 2.0M solution of BH3.DMS in THF (6.9 mL, 14.3 mmole). The reaction mixture was heated to 70° C. for 6 hours. The reaction was quenched by slow addition of methanol and stirred at room temperature for 40 minutes. The residue obtained after concentration was triturated with methanol, filtered and dried in vacuo to give 8-Bromo-2-chloro-5,6,11,12-tetrahydro-dibenzo[b,f]azocine-12-ol (0.85 g, 44%). HPLC Rt=3.31 min. m/z=338 (M+H+).

Workup

  1. customThe reaction was quenched by slow addition of methanol
  2. customThe residue obtained
  3. concentrationafter concentration
  4. customwas triturated with methanol
  5. filtrationfiltered
  6. customdried in vacuo

Sources & evidence

ORD record
ord-eb5861b5033845f9ab47dd0232a4d959
Source dataset
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07417040B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes