Acetic Acid → HCID 20445343, compound

HRID 2418780Notes

Reaction equation

HRID 2418780 reaction equation
[Cl-].[NH4+].O.C(O)(=O)C.[C:8]([O:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:25])([CH3:24])[CH2:19][C:20]([CH3:23])([CH3:22])[CH3:21])[C:15]([O:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[CH:14][C:13]=1[NH:43][S:44]([C:47]1[CH:52]=[C:51]([N+:53]([O-])=O)[CH:50]=[CH:49][C:48]=1[N:56]1[CH2:61][CH2:60][O:59][CH2:58][CH2:57]1)(=[O:46])=[O:45])(=[O:10])[CH3:9]>C(O)(C)C>[C:8]([O:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:25])([CH3:24])[CH2:19][C:20]([CH3:21])([CH3:22])[CH3:23])[C:15]([O:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[CH:14][C:13]=1[NH:43][S:44]([C:47]1[CH:52]=[C:51]([NH2:53])[CH:50]=[CH:49][C:48]=1[N:56]1[CH2:57][CH2:58][O:59][CH2:60][CH2:61]1)(=[O:45])=[O:46])(=[O:10])[CH3:9]

Participants

6

Procedure

26 g of reduced iron, 0.5 g of ammonium chloride, 7.2 ml of water and 7.2 ml of acetic acid were added to 100 ml of isopropyl alcohol and the mixture was refluxed with stirring. To the mixture was gradually added 17.5 g (0.0226 mol) of the compound obtained in Step (d) above and further refluxed with stirring for 20 minutes. After the reaction, the reaction solution was filtered with celite while hot. The filtrate was cooled and the crystals thus-precipitated were collected by filtration. Yield: 13.3 g (78%).

Workup

  1. temperaturethe mixture was refluxed
  2. temperaturefurther refluxed
  3. stirringwith stirring for 20 minutes
  4. customAfter the reaction
  5. filtrationthe reaction solution was filtered with celite while hot
  6. temperatureThe filtrate was cooled
  7. customthe crystals thus-precipitated
  8. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-4b8ca028acf04a6a928b2978bb9ee94f
Source dataset
uspto-grants-1984_09
Patent number
US04473632

Reaction notes

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