Trifluoroacetic anhydride → HCID 19609113, compound

HRID 1856846Notes

Reaction equation

HRID 1856846 reaction equation
[Cl:1][C:2]1[C:3]([CH2:11][N:12]2[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:15]([S:22](C)=O)[N:14]=[C:13]2[CH2:25][CH2:26][CH3:27])=[CH:4][C:5]2[O:9][CH2:8][O:7][C:6]=2[CH:10]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(Cl)Cl>[Cl:1][C:2]1[C:3]([CH2:11][N:12]2[C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:15]([SH:22])[N:14]=[C:13]2[CH2:25][CH2:26][CH3:27])=[CH:4][C:5]2[O:9][CH2:8][O:7][C:6]=2[CH:10]=1

Participants

4

Procedure

800 mg of the product obtained in Stage 5 above is introduced into 16 ml of methylene chloride and 0.54 ml of trifluoroacetic anhydride is added. Agitation is carried out for 30 minutes, followed by evaporating to dryness and the residue is taken up in 10 ml of methanol and 4 ml of triethylamine. Agitation is carried out for 30 minutes, followed by extraction with chloroform, washing with a saturated solution of ammonium chloride, drying and evaporating to dryness. In this way 720 mg of expected product is obtained.

Workup

  1. additionis added
  2. customby evaporating to dryness
  3. waitAgitation is carried out for 30 minutes
  4. extractionfollowed by extraction with chloroform
  5. washwashing with a saturated solution of ammonium chloride
  6. customdrying
  7. customevaporating to dryness

Sources & evidence

ORD record
ord-d73943f936c14a4d89fdd98f23c675ec
Source dataset
uspto-grants-2000_11
Patent number
US06143774

Reaction notes

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