Water → HCID 14578902, compound

HRID 231786Notes

Reaction equation

HRID 231786 reaction equation
[N:1]1[NH:2][C:3](=[O:16])[CH2:4][CH:5]2[CH2:11][CH2:10][S:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[C:6]=12.BrBr.O>C(O)(=O)C>[N:1]1[NH:2][C:3](=[O:16])[CH:4]=[C:5]2[CH2:11][CH2:10][S:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[C:6]=12

Participants

5

Reactant 3

HCID 962WaterHCID 24408BromineHCID 14578891HCID 14578891, compound

Product 1

HCID 14578902HCID 14578902, compoundYield 93.2%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To a mixture of 92 g of 4,4a,5,6-tetrahydro[1]benzothiepino[5,4-c]pyridazin-3(2H)-one in 920 ml of acetic acid is added 64 g of bromine dropwise at 50°-60° C., and the mixture is kept at the same temperature for an hour and poured into a large quantity of water. The precipitated crystals are collected by filtration, and washed with warm water and then with ethanol. The crystals are dried to give 85 g of 5,6-dihydro-[1]benzothiepino[5,4-c]pyridazin-3(2H)-one, melting at 311°-313° C. with decomposition.

Workup

  1. waitthe mixture is kept at the same temperature for an hour
  2. filtrationThe precipitated crystals are collected by filtration
  3. washwashed with warm water
  4. customThe crystals are dried

Sources & evidence

ORD record
ord-6cbd2fef96644573885393159b3beb46
Source dataset
uspto-grants-1989_07
Patent number
US04849421

Reaction notes

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