Water → HCID 14650455, compound

HRID 1200194Notes

Reaction equation

HRID 1200194 reaction equation
Br[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]#[N:21])=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[OH2:22]>>[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]([NH2:21])=[O:22])=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=1

Participants

3

Reactant 2

HCID 962WaterHCID 146504442-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran

Product 1

HCID 14650455HCID 14650455, compoundYield 57%

Conditions

Temperature
120 °C

Procedure

2-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran (3.0 g) was added to polyphosphoric acid (120 ml) and the mixture was heated on an oil bath at about 120° C. for 2 hours. After standing overnight, water (about 300 ml) was added to decompose polyphosphoric acid. Crystals deposited were filtered off and recrystallized form the mixed solvent of dichloromethane and methanol to obtain the title compound, yield 57%.

Workup

  1. filtrationCrystals deposited were filtered off
  2. customrecrystallized form the mixed solvent of dichloromethane and methanol

Sources & evidence

ORD record
ord-e6c1a28b1f2b451da736b2207e9f5ead
Source dataset
uspto-grants-1990_02
Patent number
US04904690

Reaction notes

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