HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Hydrochloric Acid → (R)-2-methyl-4,4,4-trifluorobutylamine hydrochloride

HRID 1198305
Notes
Print preview

Reaction equation

HRID 1198305 reaction equation
O.NN.[CH3:4][C@H:5]([CH2:18][C:19]([F:22])([F:21])[F:20])[CH2:6][N:7]1C(=O)C2C(=CC=CC=2)C1=O.[ClH:23]>C(O)C>[ClH:23].[CH3:4][C@H:5]([CH2:18][C:19]([F:22])([F:21])[F:20])[CH2:6][NH2:7]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 10378474(R)-2-(2-methyl-4,4,4-trifluorobutyl)-1H-isoindole-1,3(2H)-dione

Product 1

HCID 12004108(R)-2-methyl-4,4,4-trifluorobutylamine hydrochlorideYield 88%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

Hydrazine monohydrate (3.1 ml) was added to a stirred solution of (R)-2-(2-methyl-4,4,4-trifluorobutyl)-1H-isoindole-1,3(2H)-dione (17.1 g) in anhydrous ethanol (85 mL) and heated to reflux. After three hours' reflux, the solution was cooled; ethanol (40 mL) was added; and the solution was acidified to pH 1 by addition of concentrated hydrochloric acid and was filtered. The filtrate was evaporated, and the residue was purified by sublimation (bath temperature 170° C., at 6.6 Pa) to yield (R)-2-methyl-4,4,4-trifluorobutylamine hydrochloride as a white solid (9.89 g, 88%); m.p. 187°-191° C.; partial NMR (300 MHz, DMSO-d6 -D2O shake): 1.05 (d, 3H, CH3), 2.06-2.36 (m, 2H, CF3CH2) 2.36-2.54 (m, 1H, CHCH3) 2.73 (dd, 1H, CH2N), 2.87 (dd, 1H, CH2N) 8.20 (br, s, 2H, NH2).

Workup

  1. temperatureheated to reflux
  2. temperatureAfter three hours' reflux
  3. temperaturethe solution was cooled
  4. filtrationwas filtered
  5. customThe filtrate was evaporated
  6. customthe residue was purified by sublimation (bath temperature 170° C., at 6.6 Pa)

Sources & evidence

ORD record
ord-169a822bf4384dcea87206ae3094e8e1
Source dataset
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05280125

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes