Phosphorus oxychloride → HCID 57718206, compound

HRID 1984582Notes

Reaction equation

HRID 1984582 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[S:9]([NH:12][C:13]1[N:18]=[C:17](O)[C:16]([S:20][C:21]2[CH:26]=[CH:25][C:24]([S:27]([N:30]3[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]3)(=[O:29])=[O:28])=[CH:23][CH:22]=2)=[CH:15][N:14]=1)(=[O:11])=[O:10].O=P(Cl)(Cl)[Cl:38]>>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[S:9]([NH:12][C:13]1[N:18]=[C:17]([Cl:38])[C:16]([S:20][C:21]2[CH:26]=[CH:25][C:24]([S:27]([N:30]3[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]3)(=[O:29])=[O:28])=[CH:23][CH:22]=2)=[CH:15][N:14]=1)(=[O:11])=[O:10]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178527555HCID 178527555, compound

Product 1

HCID 57718206HCID 57718206, compoundYield 92.6%

Procedure

A solution of 10 (150 mg, 0.26 mmol) in POCl3 (0.24 mL, 2.6 mmol) was heated to 90° C. for 3.5 hours. The mixture was cooled to room temperature and poured onto ice. The precipitate was collected by filtration, washed with water and dried under vacuum to afford 11 as a pale yellow solid (143 mg), which was used without further purification. Mass Spectrum m/e=594.8 (M+1)

Workup

  1. additionpoured onto ice
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customdried under vacuum

Sources & evidence

ORD record
ord-7e49b98ee8874051a6ecee0eb15c46c5
Source dataset
uspto-grants-2009_06
Patent number
US07544702B2

Reaction notes

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