Hydrochloric Acid → HCID 118193100, compound

HRID 2199528Notes

Reaction equation

HRID 2199528 reaction equation
O[CH2:2][CH2:3][NH:4][C@H:5]([C:8]([OH:10])=[O:9])[CH2:6][SH:7].[ClH:11]>>[ClH:11].[Cl:11][CH2:2][CH2:3][NH:4][C@H:5]([C:8]([OH:10])=[O:9])[CH2:6][SH:7]

Participants

3

Procedure

44 g of 2-hydroxyethyl cysteine was added into a 1000 ml round-bottom flask, dissolved in 600 ml of concentrated hydrochloric acid, heated till the external temperature was 90-95° C., stirred and reacted for 7 h. After the reaction, the system was refrigerated and left to stand overnight, and a large number of needle-like solid was precipitated from the system. The solvent was removed by sucking filtration, the obtained solid was naturally dried to give a gray white solid wherein the mp is 185-186° C., the weight is about 40 g, and the yield is more than 70%. 1H-NMR (400 MHz, D2O) δ: 4.30477-4.26952 (m, 1H), 3.81913-3.78409 (m, 2H), 3.25903 (dd, 1H, J1=4.444 Hz, J2=14.984 Hz), 3.18877 (dd, 1H, J1=7.352 Hz, J2=15.072 Hz), 3.04410-3.00625 (m, 2H).

Workup

  1. temperatureheated till the external temperature
  2. customwas 90-95° C.
  3. customreacted for 7 h
  4. customAfter the reaction
  5. waitleft
  6. customa large number of needle-like solid was precipitated from the system
  7. customThe solvent was removed
  8. filtrationfiltration
  9. customthe obtained solid was naturally dried
  10. customto give a gray white solid wherein the mp is 185-186° C.

Sources & evidence

ORD record
ord-439253e599124d31a21acb73b78933ab
Source dataset
uspto-grants-2016_06
Patent number
US09359314B2

Reaction notes

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