Acetonitrile → HCID 135736170, compound

HRID 4251Notes

Reaction equation

HRID 4251 reaction equation
[C:1]([C:3]1[NH:4][N:5]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[CH3:29])[C:6](=[O:22])[C:7]=1[N:8]=[N:9][C:10]1[CH:15]=[C:14]([CH3:16])[C:13]([S:17](O)(=[O:19])=[O:18])=[CH:12][C:11]=1[CH3:21])#[N:2].C(#N)C.P(Cl)(Cl)([Cl:35])=O>CN(C)C(=O)C>[Cl:35][S:17]([C:13]1[C:14]([CH3:16])=[CH:15][C:10]([N:9]=[N:8][C:7]2[C:6](=[O:22])[N:5]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[CH3:29])[NH:4][C:3]=2[C:1]#[N:2])=[C:11]([CH3:21])[CH:12]=1)(=[O:19])=[O:18]

Participants

5

Procedure

8.6 g of the azo obtained in step (2) above, 35 ml of acetonitrile, and 8.6 ml of N,N-dimethylacetamide were put into a 100 ml three-necked flask and 8.6 ml of phosphorus oxychloride was added dropwise to the mixture at a temperature of 50° C. or below. After completion of the dropwise addition, the mixture was stirred for 30 minutes and then poured into ice water. The crystals thus deposited were collected by filtration.

Workup

  1. additionAfter completion of the dropwise addition
  2. filtrationThe crystals thus deposited were collected by filtration

Sources & evidence

ORD record
ord-b37197377f3049a1b8bb4c506a8c3f2c
Source dataset
uspto-grants-1988_02
Patent number
US04725531

Reaction notes

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