Acetic Anhydride → HCID 21243163, compound

HRID 621425

Reaction equation

HRID 621425 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:9][CH:10]2[CH2:12][CH2:11]2)[N:3]=1.C(N(CC)CC)C.[C:20](OC(=O)C)(=[O:22])[CH3:21]>O1CCCC1>[CH:10]1([NH:9][C:4]2[N:3]=[C:2]([NH:1][C:20](=[O:22])[CH3:21])[N:7]=[C:6]([NH2:8])[N:5]=2)[CH2:12][CH2:11]1

Participants

5

Reactant 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 47866Cyromazine

Product 1

HCID 21243163HCID 21243163, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

To a suspension of 49.8 g of 2,4-diamino-6-cyclopropylamino-1,3,5-triazine and 45.5 g of triethylamine in 1200 ml of tetrahydrofuran are slowly added dropwise, at about 60° C. (in about 6 hours), 31.7 g of acetic acid anhydride dissolved in 100 ml of tetrahydrofuran. The reaction mixture is subsequently refluxed for 18 hours, filtered hot and then concentrated by evaporation until crystallisation commences. After the addition of about 300 ml of diethyl ether, the product if filtered off as white crystalline powder. It has a melting point of 190°-195° C.

Workup

  1. temperatureThe reaction mixture is subsequently refluxed for 18 hours
  2. filtrationfiltered hot
  3. concentrationconcentrated by evaporation until crystallisation commences
  4. additionAfter the addition of about 300 ml of diethyl ether
  5. filtrationthe product if filtered off as white crystalline powder

Sources & evidence

ORD record
ord-6b903e07e5bc49d982a83da5f239842c
Source dataset
uspto-grants-1989_04
Patent number
US04824845

Linked notes

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