4-Chloro-1-butanol → HCID 69054781, compound

HRID 1453663Notes

Reaction equation

HRID 1453663 reaction equation
[N:1]([C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]=1[CH3:13])=[C:2]=[O:3].[Cl:14][CH2:15][CH2:16][CH2:17][CH2:18][OH:19]>C1(C)C=CC=CC=1>[CH3:13][C:5]1[CH:6]=[C:7]([N+:10]([O-:12])=[O:11])[CH:8]=[CH:9][C:4]=1[NH:1][C:2](=[O:3])[O:19][CH2:18][CH2:17][CH2:16][CH2:15][Cl:14]

Participants

4

Reactant 2

HCID 135694-Chloro-1-butanolHCID 42964562-Methyl-4-nitrophenyl isocyanate

Product 1

HCID 69054781HCID 69054781, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

17.8 g (0.10 mol) 4-isocyanato-3-methyl-1-nitro-benzene are placed in 750 ml of toluene and a solution of 11.7 ml (0.10 mol) 4-chloro-butan-1-ol in 50 ml of toluene is added dropwise. Then the reaction mixture is heated for 16 hours to 75° C., then evaporated down i. vac. and twice taken up with toluene and concentrated by evaporation completely i. vac. The residue is purified by recrystallisation from cyclohexane.

Workup

  1. temperatureThen the reaction mixture is heated for 16 hours to 75° C.
  2. customevaporated down i
  3. concentrationconcentrated by evaporation
  4. customThe residue is purified by recrystallisation from cyclohexane

Sources & evidence

ORD record
ord-c739a30a17c14ce2bc65c1fc0de2d3f7
Source dataset
uspto-grants-2009_01
Patent number
US07476663B2

Reaction notes

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