Ethylenediamine → HCID 21472721, compound

HRID 1736473Notes

Reaction equation

HRID 1736473 reaction equation
[C:1]([O:5][C:6]([N:8]1[C:12]2[C:13]([F:21])=[CH:14][C:15]([N:18]=[C:19]=[S:20])=[C:16]([CH3:17])[C:11]=2[N:10]=[CH:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:22]([NH2:25])[CH2:23][NH2:24]>C(Cl)Cl>[C:1]([O:5][C:6]([N:8]1[C:12]2[C:13]([F:21])=[CH:14][C:15]([NH:18][C:19]([NH:24][CH2:23][CH2:22][NH2:25])=[S:20])=[C:16]([CH3:17])[C:11]=2[N:10]=[CH:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

Participants

4

Reactant 2

HCID 3301EthylenediamineHCID 21472729HCID 21472729, compound

Product 1

HCID 21472721HCID 21472721, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A solution of 1-tert-butoxycarbonyl-7-fluoro-4-methyl-5-benzimidazolylisothiocyanate (0.42 g) in methylene chloride (50 mL) is added dropwise over 15 minutes to 1,2-ethylenediamine (0.45 mL) in solution in methylene chloride (100 mL). The mixture is stirred for 10 minutes at room temperature, then rotary evaporated. The residue is triturated for 30 minutes with ether (100 mL). The resulting white suspension is filtered and the solid is dried in vacuo overnight.

Workup

  1. customThe residue is triturated for 30 minutes with ether (100 mL)
  2. filtrationThe resulting white suspension is filtered
  3. customthe solid is dried in vacuo overnight

Sources & evidence

ORD record
ord-3e316eac530f430196c7f84b17d9600a
Source dataset
uspto-grants-1996_07
Patent number
US05541210

Reaction notes

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