Water → HCID 178441902, compound

HRID 2260822Notes

Reaction equation

HRID 2260822 reaction equation
[N+:1]([O-])([O-])=O.[Na+].[C:6]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18])#[C:7][CH2:8][CH2:9][CH2:10][CH3:11].[OH2:19]>Cl>[CH2:8]([C:7]1[N:1]=[N:18][C:13]2[C:12]([C:6]=1[OH:19])=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:9][CH2:10][CH3:11]

Participants

5

Reactant 3

HCID 962Water2×HCID 24268Sodium NitrateHCID 107973102-(Hex-1-yn-1-yl)aniline

Product 1

HCID 178441902HCID 178441902, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
0 °C

Procedure

A solution of 2 g of sodium nitrate in 60 ml of water was added at 0° C. to a suspension at 0° C. of 3.2 g of the product of Step A in 100 ml of concentrated hydrochloric acid. The mixture was stirred for 90 minutes at 0° C., then for one hour at 100° C. The reaction medium was poured into 100 ml of ice-cooled water, followed by separating and washing with ice-cooled water. The moist product was taken up in 100 ml of water and alkalized with concentrated ammonium hydroxide. After separating, the residue was washed with water and dried at 70° C. under reduced pressure to obtain 1.47 g of the expected product melting at 180° C.

Workup

  1. waitfor one hour at 100° C
  2. customby separating
  3. washwashing with ice-
  4. temperaturecooled water
  5. customAfter separating
  6. washthe residue was washed with water
  7. customdried at 70° C. under reduced pressure

Sources & evidence

ORD record
ord-badd5a379a394324b0b30870000e5e47
Source dataset
uspto-grants-1995_12
Patent number
US05478938

Reaction notes

Loading…