Acetic Acid → HCID 20292403, compound

HRID 1413538Notes

Reaction equation

HRID 1413538 reaction equation
[C:1]([O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:7][C:6]=1[NH:29][S:30]([C:33]1[CH:38]=[C:37]([N+:39]([O-])=O)[CH:36]=[CH:35][C:34]=1[N:42]1[CH2:47][CH2:46][O:45][CH2:44][CH2:43]1)(=[O:32])=[O:31])(=[O:3])[CH3:2].[Cl-].[NH4+].O.C(O)(=O)C>C(O)(C)C>[C:1]([O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:7][C:6]=1[NH:29][S:30]([C:33]1[CH:38]=[C:37]([NH2:39])[CH:36]=[CH:35][C:34]=1[N:42]1[CH2:43][CH2:44][O:45][CH2:46][CH2:47]1)(=[O:31])=[O:32])(=[O:3])[CH3:2]

Participants

6

Reactant 4

HCID 176Acetic AcidHCID 962WaterHCID 25517Ammonium ChlorideHCID 70514192HCID 70514192, compound

Product 1

HCID 20292403HCID 20292403, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

19.5 g (0.029 mol) of the compound obtained in Step (c) above, reduced iron (5.3 g), triirontetraoxide (2.7 g) and ammonium chloride (0.4 g) were suspended in isopropanol (300 ml). To the mixture, a mixed solution of water (40 ml) and acetic acid (2 ml) was added dropwise while refluxing with heating. After the completion of the addition, the mixture was refluxed wih heating for 2 hours and the insoluble materials were removed by filtration while hot. The filtrate was added to water (300 ml) and the crystals thus-precipitated were collected by filtration. Yield: 16.4 g (86%). Melting Point: 110°-112° C.

Workup

  1. temperaturewhile refluxing
  2. temperaturewith heating
  3. additionAfter the completion of the addition
  4. temperaturethe mixture was refluxed wih
  5. temperatureheating for 2 hours
  6. customthe insoluble materials were removed by filtration while hot
  7. additionThe filtrate was added to water (300 ml)
  8. customthe crystals thus-precipitated
  9. filtrationwere collected by filtration

Sources & evidence

ORD record
ord-6a47fadb76274c7a990a1438f965271b
Source dataset
uspto-grants-1981_02
Patent number
US04250246

Reaction notes

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