Water → HCID 67064832, compound

HRID 1392807Notes

Reaction equation

HRID 1392807 reaction equation
Cl[C:2]1[CH:8]=[CH:7][C:5](O)=[CH:4][C:3]=1[OH:9].[Cl:10][C:11]1[CH:12]=[C:13]2[C:18](=O)OC(=O)[C:14]2=[CH:20][C:21]=1[Cl:22].O>CS(O)(=O)=O>[Cl:22][C:21]1[C:11]([Cl:10])=[C:12]([C:2]2[CH:8]=[CH:7][CH:5]=[CH:4][CH:3]=2)[C:13]2[CH2:18][C:4]3[C:3]([O:9][C:14]=2[CH:20]=1)=[CH:2][CH:8]=[CH:7][CH:5]=3

Participants

5

Reactant 3

HCID 962WaterHCID 17314-ChlororesorcinolHCID 703344,5-Dichlorophthalic anhydride

Product 1

HCID 67064832HCID 67064832, compound

Reagents, catalysts & solvents 1

HCID 6395Methanesulfonic AcidSolvent

Conditions

Temperature
180 °C

Procedure

4-Chlororesorcinol (33 g) was mixed with 4,5-dichlorophthalic anhydride in methane sulfonic acid (100 mL) according to the procedure of Menchen, et. al, (U.S. Pat. No. 5,654,442). Briefly, with magnetic stirring, the solution was heated to 180° C. over 30 min and maintained for an additional 30 minutes. The mixture was allowed to cool to ˜100° C. and was cautiously poured into water (1 L). The solid was collected by filtration and air dried for several days, followed by 24 h of high vacuum and was characterized as having the structure above.

Workup

  1. temperaturemaintained for an additional 30 minutes
  2. temperatureto cool to ˜100° C.
  3. filtrationThe solid was collected by filtration and air
  4. customdried for several days

Sources & evidence

ORD record
ord-962c37a08c73483f85074fea064b0387
Source dataset
uspto-grants-2008_03
Patent number
US07344701B2

Reaction notes

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