Acetonitrile → HCID 135736170, compound
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
Reactant 3
Product 1
Reagents, catalysts & solvents 1
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
- additionAfter completion of the dropwise addition
- 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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