Methyl Isocyanate → HCID 20262406, compound

HRID 464630Notes

Reaction equation

HRID 464630 reaction equation
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]1[C:14]([C:15]([O:17][CH3:18])=[O:16])=[C:13]([CH3:19])[NH:12][C:11]([CH2:20][O:21][CH2:22][C:23]2[N:24]=[N:25][N:26]([CH2:28][CH2:29][N:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)[N:27]=2)=[C:10]1[C:36]([O:38][CH2:39][CH3:40])=[O:37].[CH3:41][N:42]=[C:43]=[O:44]>ClCCl>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]1[C:14]([C:15]([O:17][CH3:18])=[O:16])=[C:13]([CH3:19])[NH:12][C:11]([CH2:20][O:21][CH2:22][C:23]2[N:24]=[N:25][N:26]([CH2:28][CH2:29][N:30]3[CH2:35][CH2:34][N:33]([C:43](=[O:44])[NH:42][CH3:41])[CH2:32][CH2:31]3)[N:27]=2)=[C:10]1[C:36]([O:38][CH2:39][CH3:40])=[O:37]

Participants

4

Reactant 2

HCID 12228Methyl IsocyanateHCID 20262405HCID 20262405, compound

Product 1

HCID 20262406HCID 20262406, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of 5-{[4-(2,3-dichlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-2-[2-(1-piperazinyl)ethyl]tetrazole (321 mg) and methyl isocyanate (0.5 ml) in dichloromethane (10 ml) was stirred at room temperature for 30 minutes and evaporated. The residual oil was triturated with diethyl ether and the resulting solid collected, washed with diethyl ether and dried to give the title compound as a hemihydrate (383 mg), m.p. 112°-114° C. Found: C,50.78; H,5.59; N,16.89. C26H33Cl2N7O5.0.5H2O requires: C,50.91; H,5.60; N,16.96%.

Workup

  1. customevaporated
  2. customThe residual oil was triturated with diethyl ether
  3. customthe resulting solid collected
  4. washwashed with diethyl ether
  5. customdried

Sources & evidence

ORD record
ord-a26d9ab3536b4649a4a53bcb786d29f8
Source dataset
uspto-grants-1985_10
Patent number
US04548935

Reaction notes

Loading…