Hydrochloric Acid → HCID 67847844, compound

HRID 2073448Notes

Reaction equation

HRID 2073448 reaction equation
[CH2:1]([NH:10][C@H:11]1[CH2:16][CH2:15][C@H:14]2[C@H:17]3[C@H:26]([CH2:27][CH2:28][C@:12]12[CH3:13])[C:25]1[CH:24]=[CH:23][C:22]([O:29][CH3:30])=[CH:21][C:20]=1[CH2:19][CH2:18]3)[CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][CH2:8][NH2:9].[ClH:31].C(OCC)C>CO>[ClH:31].[ClH:31].[ClH:31].[CH2:1]([NH:10][C@H:11]1[CH2:16][CH2:15][C@H:14]2[C@H:17]3[C@H:26]([CH2:27][CH2:28][C@:12]12[CH3:13])[C:25]1[CH:24]=[CH:23][C:22]([O:29][CH3:30])=[CH:21][C:20]=1[CH2:19][CH2:18]3)[CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][CH2:8][NH2:9]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 67847835HCID 67847835, compound

Product 1

HCID 67847844HCID 67847844, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

A solution of the title compound from Example 94, (0.17 g) in absolute methanol (1 ml) is treated at 20°-25° under argon with 0.53M anhydrous HCl in methanol (2.8 ml) until acidic by pH paper. The resulting solution is stirred for ~ 5 minutes at 20°-25°, treated with anhydrous diethyl ether (45 ml) over 30 minutes, and the resulting suspension is stirred for 15 minutes under argon. The suspension is filtered, and the filtercake is washed with anhydrous ether (~ 15 ml). The light yellow powder is dried under high vacuum overnight to give the title compound, mp 230°-235° C. (PLA2)

Workup

  1. stirringthe resulting suspension is stirred for 15 minutes under argon
  2. filtrationThe suspension is filtered
  3. washthe filtercake is washed with anhydrous ether (~ 15 ml)
  4. customThe light yellow powder is dried under high vacuum overnight

Sources & evidence

ORD record
ord-6d288745a0004325908db223e37e1240
Source dataset
uspto-grants-1990_04
Patent number
US04917826

Reaction notes

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