Acetic Acid → HCID 13983508, compound
Reaction equation
Cl[S:2]([C:5]1[CH:6]=[C:7]([C:15]([OH:17])=[O:16])[C:8]2[O:12][CH:11]([CH3:13])[CH2:10][C:9]=2[CH:14]=1)(=O)=O.C(O)(=O)C.[Sn].Cl>O>[SH:2][C:5]1[CH:6]=[C:7]([C:15]([OH:17])=[O:16])[C:8]2[O:12][CH:11]([CH3:13])[CH2:10][C:9]=2[CH:14]=1Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
216 g of 5-chlorosulphonyl-2-methyl-2,3,-dihydrobenzofuran-7-carboxylic acid, 585 ml of acetic acid and 348 g of tin were introduced into a 6-liter round-bottomed flask and 1560 ml of concentrated hydrochloric acid (d =1.18) were then added dropwise, while maintaining the temperature between 45° and 55° C. The contents were then heated for 2 hours at 55°-60° C. until the tin was completely dissolved, and the solution which was poured into 12 liters of water was then filtered. The crystals formed were drained, washed with water and dried at 40° C.
Workup
- temperaturewhile maintaining the temperature between 45° and 55° C
- dissolutionwas completely dissolved
- filtrationwas then filtered
- customThe crystals formed
- washwashed with water
- customdried at 40° C.
Sources & evidence
- ORD record
- ord-590554103c9b43d799158b3dc305a590
- Source dataset
- uspto-grants-1991_04
- Patent number
- US05006570
Reaction notes
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