Carbon Tetrachloride → HCID 15278640, compound

HRID 129385Notes

Reaction equation

HRID 129385 reaction equation
[F:1][C:2]1[C:15]([NH:16][C:17](=O)[CH2:18][Cl:19])=[CH:14][C:5]2[N:6]([CH2:11][C:12]#[CH:13])[C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:41]>ClCCCl>[F:1][C:2]1[C:15]([N:16]=[C:17]([Cl:41])[CH2:18][Cl:19])=[CH:14][C:5]2[N:6]([CH2:11][C:12]#[CH:13])[C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1

Participants

5

Reactant 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 19371415HCID 19371415, compound

Product 1

HCID 15278640HCID 15278640, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Procedure

First, 1.00 g of N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-2-chloroacetamide, 2.25 g of triphenylphosphine polymer bound and 4 ml of carbon tetrachloride were dissolved in 35 ml of 1,2-dichloroethane, and then the reflux under heat was continued for 2 hr. After letting the solution stand to cool the same, the solid was filtered out, and then the solvent was distilled out under reduced pressure to quantitatively obtain N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-2-chloroacetimidoylchloride.

Workup

  1. temperaturethe reflux
  2. temperatureunder heat
  3. temperatureto cool the same, the solid
  4. filtrationwas filtered out
  5. distillationthe solvent was distilled out under reduced pressure to quantitatively obtain N-(7-fluoro-4-propargyl-2H-1,4-benzoxazine-3(4H)-one-6-yl)-2-chloroacetimidoylchloride

Sources & evidence

ORD record
ord-6a0f5a761eb1447c9f3563ecd92164b9
Source dataset
uspto-grants-1995_11
Patent number
US05468719

Reaction notes

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