Water → HCID 58124873, compound

HRID 1971708Notes

Reaction equation

HRID 1971708 reaction equation
[C:1]([O:5][C:6]([N:8]([CH2:38][C:39]#[C:40][C:41]1[S:42][CH:43]=[CH:44][CH:45]=1)[CH2:9][CH2:10][N:11]([CH:35]([CH3:37])[CH3:36])[C:12](=[O:34])[C:13]([N:15]1[CH2:24][CH2:23][C:22]2[C:17](=[CH:18][C:19]([O:27][CH:28]([CH3:30])[CH3:29])=[C:20]([O:25][CH3:26])[CH:21]=2)[CH:16]1C(O)=O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[Na+].O>C(OC(=O)C)(=O)C>[CH:35]([N:11]1[C:12](=[O:34])[C:13]2[N:15]3[CH2:24][CH2:23][C:22]4[CH:21]=[C:20]([O:25][CH3:26])[C:19]([O:27][CH:28]([CH3:29])[CH3:30])=[CH:18][C:17]=4[C:16]3=[C:40]([C:41]3[S:42][CH:43]=[CH:44][CH:45]=3)[C:39]=2[CH2:38][N:8]([C:6]([O:5][C:1]([CH3:3])([CH3:4])[CH3:2])=[O:7])[CH2:9][CH2:10]1)([CH3:36])[CH3:37]

Participants

5

Reactant 3

HCID 962WaterHCID 517045Sodium AcetateHCID 58124889HCID 58124889, compound

Product 1

HCID 58124873HCID 58124873, compoundYield 80.2%

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of 580 mg of 14c and 1 g of anhydrous sodium acetate in 8 ml of acetic anhydride was heated at 100° C. for 45 min. The reaction mixture was cooled and 25 ml of water was added and stirring prolonged for 1 h. The product crystallized from the reaction mixture and was filtered, washed with water and dried in vacuo, to give 420 mg of 14d as white crystalline material; Mp 205-206° C.

Workup

  1. temperatureThe reaction mixture was cooled
  2. customThe product crystallized from the reaction mixture
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried in vacuo

Sources & evidence

ORD record
ord-aaff33feec1445cabdf1ba1b8f317195
Source dataset
uspto-grants-2013_04
Patent number
US08431564B2

Reaction notes

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