Hydrochloric Acid → HCID 57475101, compound

HRID 1095479Notes

Reaction equation

HRID 1095479 reaction equation
Cl.[S:2]1[C:6]([C:7]2([N:17]([CH3:19])[CH3:18])[CH2:16][CH2:15][C:10]3(OCC[O:11]3)[CH2:9][CH2:8]2)=[CH:5][C:4]2[CH:20]=[CH:21][CH:22]=[CH:23][C:3]1=2.Cl>O>[S:2]1[C:6]([C:7]2([N:17]([CH3:18])[CH3:19])[CH2:16][CH2:15][C:10](=[O:11])[CH2:9][CH2:8]2)=[CH:5][C:4]2[CH:20]=[CH:21][CH:22]=[CH:23][C:3]1=2

Participants

4

Procedure

(8-Benzo[b]thiophen-2-yl-1,4-dioxa-spiro[4.5]dec-8-yl)-dimethyl-amine hydrochloride (0.60 g, 1.7 mmol) was dissolved in water (0.8 ml), concentrated hydrochloric acid (1.04 ml, 151 mmol) was added and the mixture was stirred at room temperature for 3 d. When the hydrolysis had ended, the reaction mixture was extracted with diethyl ether (2×25 ml) and the aqueous phase was rendered alkaline with 5 N sodium hydroxide solution, the mixture was extracted with methylene chloride (3×25 ml) and the extract was dried over sodium sulfate and concentrated i. vac. Yield: 0.44 g (95%) Ket-6

Workup

  1. extractionthe reaction mixture was extracted with diethyl ether (2×25 ml)
  2. extractionthe mixture was extracted with methylene chloride (3×25 ml)
  3. dry with materialthe extract was dried over sodium sulfate
  4. concentrationconcentrated i

Sources & evidence

ORD record
ord-2cdcf05b3a7e482abde6c69597d1350f
Source dataset
uspto-grants-2012_03
Patent number
US08138187B2

Reaction notes

Loading…