Hydrochloric Acid → HCID 13472262, compound

HRID 483064Notes

Reaction equation

HRID 483064 reaction equation
CC([NH:5][S:6]([C:9]1[C:10]2[CH2:11][N:12]([CH3:18])[CH2:13][C:14]=2[CH:15]=[CH:16][CH:17]=1)(=[O:8])=[O:7])(C)C.B.[ClH:20]>CO>[ClH:20].[CH3:18][N:12]1[CH2:11][C:10]2[C:9]([S:6]([NH2:5])(=[O:8])=[O:7])=[CH:17][CH:16]=[CH:15][C:14]=2[CH2:13]1

Participants

4

Procedure

A suspension of 5.3 g of the compound prepared in Example 16 in 20 ml of methanol was cooled to 10° and 50 ml of concentrated hydrochloric acid was added dropwise at 10°-15° (gas evolution). The reaction mixture was allowed to warm to room temperature and then refluxed 3.75 hours. The reaction solution was cooled and concentrated in vacuo. The white solid was washed with ethanol followed by ethyl acetate then dried to give 4.1 g of 2,3-dihydro-2-methyl-1H-isoindole-4-sulfonamide hydrochloride, m.p. >250°.

Workup

  1. temperaturewas cooled to 10°
  2. temperaturerefluxed 3.75 hours
  3. temperatureThe reaction solution was cooled
  4. concentrationconcentrated in vacuo
  5. washThe white solid was washed with ethanol
  6. customthen dried

Sources & evidence

ORD record
ord-59267c40b5d14771897abd615e55ae1f
Source dataset
uspto-grants-1986_03
Patent number
US04578108

Reaction notes

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