Benzyl Chloride → 2-(Benzylsulfanyl)ethan-1-amine

HRID 1781165Notes

Reaction equation

HRID 1781165 reaction equation
Cl.[NH2:2][CH2:3][CH2:4][SH:5].[CH2:6](Cl)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C(OCC)(=O)C>[CH2:6]([S:5][CH2:4][CH2:3][NH2:2])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Participants

6

Procedure

A suspension of 2-aminoethanethiol hydrochloride (2.27 g, 20.0 mmol), benzyl chloride (2.42 mL, 21.0 mmol) and cesium carbonate (19.5 g, 60 mmol) in DMF (100 mL) was stirred overnight. The reaction mixture was then diluted with ethyl acetate (200 mL) and filtered into a separation funnel. The solid residue was washed with ether (50 mL×3). The combined filtrates were then washed with water (80 mL×5) and brine (50 mL), dried over potassium carbonate and filtered. The filtrate was concentrated first with rotary evaporator (water bath at 80° C.), then by high vacuum (1 mm Hg) to give 2-benzylthioethylamine in good purity. The crude product was used for next step without further purification.

Workup

  1. filtrationfiltered into a separation funnel
  2. washThe solid residue was washed with ether (50 mL×3)
  3. washThe combined filtrates were then washed with water (80 mL×5) and brine (50 mL)
  4. dry with materialdried over potassium carbonate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated first with rotary evaporator (water bath at 80° C.)

Sources & evidence

ORD record
ord-bd793c39aa344d96bb53fd572d791e4d
Source dataset
uspto-grants-1997_05
Patent number
US05631401

Reaction notes

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