Water → HCID 178450603, compound

HRID 355017Notes

Reaction equation

HRID 355017 reaction equation
[CH:1]1[C:6]2[C:7]3[C:15](=[O:16])[O:14][C:12](=[O:13])[C:8]=3[CH2:9][CH2:10][CH2:11][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:17][C:18]([CH3:23])([CH2:21][NH2:22])[CH2:19][OH:20].O>C1(C)C=CC=CC=1>[OH:20][CH2:19][C:18]([CH3:23])([CH3:17])[CH2:21][N:22]=[C:12]([C:8]1[CH2:9][CH2:10][CH2:11][C:5]2[CH:4]=[CH:3][CH:2]=[CH:1][C:6]=2[C:7]=1[C:15]([OH:14])=[O:16])[OH:13]

Participants

5

Reactant 3

HCID 962WaterHCID 1173261-Propanol, 3-amino-2,2-dimethyl-HCID 54435650HCID 54435650, compound

Product 1

HCID 178450603HCID 178450603, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

21.4 g (0.1 mol) of 6,7-dihydro-5H-benzocycloheptene-8,9-dicarboxylic acid anhydride and 10.3 g (0.1 mol) of 2,2-dimethyl-3-aminopropanol are dissolved in 60 ml of toluene and the solution is refluxed for 1 hour, the water formed being separated off by means of a water separator downstream of the reaction vessel. After cooling to room temperature, the crystals which have precipitated out are filtered off. This yields 28.9 g (96.6% of theory) of N-(3'-hydroxy-2',2'-dimethylpropyl)-6,7-dihydro-5H-benzocycloheptene-8,9-dicarboxylic acid imide.

Workup

  1. temperaturethe solution is refluxed for 1 hour
  2. custombeing separated off by means of a water separator downstream of the reaction vessel
  3. customthe crystals which have precipitated out
  4. filtrationare filtered off

Sources & evidence

ORD record
ord-d9c687c52cd84546bba7ec2153ffdddc
Source dataset
uspto-grants-1983_03
Patent number
US04377669

Reaction notes

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