1-Ethoxyethanol → HCID 135476600, compound

HRID 1350348Notes

Reaction equation

HRID 1350348 reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]([C:14]3[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][C:15]=3[OH:21])[N:11]=[C:10]([C:22]3[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][C:23]=3[OH:29])[N:9]=2)=[CH:4][CH:3]=1.C(O[CH:33]([OH:35])[CH3:34])C>[Cl-].C([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)C1C=CC=CC=1>[OH:1][CH2:2][CH2:3][O:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[C:10]([C:22]3[CH:27]=[CH:26][C:25]([O:28][CH2:16][CH2:17][OH:20])=[CH:24][C:23]=3[OH:29])[N:11]=[C:12]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH2:34][CH2:33][OH:35])=[CH:16][C:15]=3[OH:21])[N:13]=2)=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 101298981-EthoxyethanolHCID 136351974HCID 136351974, compound

Product 1

HCID 135476600HCID 135476600, compound

Reagents, catalysts & solvents 1

HCID 70671Benzyltriphenylphosphonium chlorideCatalyst

Conditions

Temperature
100 °C

Procedure

2-[4-Hydroxyphenyl)-4,6-bis-(2,4-dihydroxyphenyl)-1,3,5-triazine (10 g) is suspended in 100 ml 2 ethoxyethanol and heated to 100° C. Benzyltriphenylphosphonium chloride (0.12 g) is added followed by ethylenecarbonate (8.59 g) over a period of 7 hours. The reaction mixture is stirred at 135° C. for 10 hours then cooled to RT. The crystals are filtered off, washed with 100 ml cold methanol and 100 ml cold water and dried under reduced pressure. The title compound (9.0 g) is obtained with mp 169° C.

Workup

  1. temperaturethen cooled to RT
  2. filtrationThe crystals are filtered off
  3. washwashed with 100 ml cold methanol and 100 ml cold water
  4. customdried under reduced pressure

Sources & evidence

ORD record
ord-7bd8059f04344fa0bdc51e1ed034e336
Source dataset
uspto-grants-2007_05
Patent number
US07214742B2

Reaction notes

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