Water → HCID 702159, compound

HRID 1376585Notes

Reaction equation

HRID 1376585 reaction equation
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1.C(N(CC)CC)C.[C:25](Cl)(=[O:27])[CH3:26].O>O1CCCC1>[C:25]([O:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[N:9]1[N:13]=[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]2=[N:10]1)(=[O:27])[CH3:26]

Participants

6

Reactant 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 17113Drometrizole

Product 1

HCID 702159HCID 702159, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

2-(2'-Hydroxy-5-methylphenyl)2H-benzotriazole(Tinuvin P manufactured by Ciba Geigy Co., Ltd., λmax=336 nm) 1.13 part and triethylamine 0.61 part were dissolved in acetonitrile 20 parts. A solution of acetyl chloride 0.43 part/acetonitrile 10 parts was dropped thereto while cooling with ice. After stirring at a room temperature for further 4 hours, the solution was poured into water 200 parts and extracted with chloroform, followed by condensing and refining with recrystallization (isopropyl alcohol/chloroform). A pale yellow crystal 0.9 part of 2-(2'-acetoxy-5-methylphenyl)2H-benzotriazole was obtained. (λmax=298 nm).

Workup

  1. temperaturewhile cooling with ice
  2. extractionextracted with chloroform
  3. customfollowed by condensing
  4. customrefining with recrystallization (isopropyl alcohol/chloroform)

Sources & evidence

ORD record
ord-50477b31110c4a41ab61b5175f6714df
Source dataset
uspto-grants-1997_09
Patent number
US05663212

Reaction notes

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