Phosphorus oxychloride → HCID 18929616, compound

HRID 1080647Notes

Reaction equation

HRID 1080647 reaction equation
O[C:2]1[C:11]2[CH:12]=[C:13]([O:15][CH3:16])[CH:14]=[C:9]3[C:10]=2[N:5]([CH2:6][CH2:7][O:8]3)[C:4](=[O:17])[C:3]=1[C:18]([N:20]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22][CH2:21]1)=[O:19].P(Cl)(Cl)([Cl:31])=O>>[Cl:31][C:2]1[C:11]2[CH:12]=[C:13]([O:15][CH3:16])[CH:14]=[C:9]3[C:10]=2[N:5]([CH2:6][CH2:7][O:8]3)[C:4](=[O:17])[C:3]=1[C:18]([N:20]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22][CH2:21]1)=[O:19]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 54710159HCID 54710159, compound

Product 1

HCID 18929616HCID 18929616, compound

Conditions

Temperature
80 °C

Procedure

A mixture of 2,3-dihydro-7-hydroxy-9-methoxy-6-(1-indolinylcarbonyl)-5-oxo-5H-pyrido[1,2,3-de]-1,4-benzoxazine (3 g) and phosphorus oxychloride (2.2 ml) was stirred at 80° C. for 1 hour. The mixture was poured into ice-water and the precipitates were collected and washed with water to give yellow crystals of 2,3-dihydro-7-chloro-9-methoxy-6-(1-indolinylcarbonyl)-5-oxo-5H-pyrido[1,2,3-de]-1,4-benzoxazine (2.8 g).

Workup

  1. customthe precipitates were collected
  2. washwashed with water

Sources & evidence

ORD record
ord-9749fe07a4684f44a85676d1428997ed
Source dataset
uspto-grants-1996_12
Patent number
US05583135

Reaction notes

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