Water → HCID 14851855, compound

HRID 1032758Notes

Reaction equation

HRID 1032758 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16](I)[CH:17]=[CH:18][C:13]=2[N:12]2[C:20]([CH3:23])=[N:21][N:22]=[C:11]2[CH2:10][N:9]=1.[CH3:24][N:25]1[C:31](=[O:32])[C:30]2[CH:33]=[CH:34][CH:35]=[CH:36][C:29]=2[N:28]([CH2:37][C:38]#[CH:39])[C:27](=[O:40])[CH2:26]1.C(OCC)(=O)C.O.C#C>>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([C:39]#[C:38][CH2:37][N:28]3[C:29]4[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=4[C:31](=[O:32])[N:25]([CH3:24])[CH2:26][C:27]3=[O:40])[CH:17]=[CH:18][C:13]=2[N:12]2[C:20]([CH3:23])=[N:21][N:22]=[C:11]2[CH2:10][N:9]=1

Participants

6

Reactant 5

HCID 962WaterHCID 6326AcetyleneHCID 8857Ethyl AcetateHCID 14851835HCID 14851835, compoundHCID 14851944HCID 14851944, compound

Product 1

HCID 14851855HCID 14851855, compound

Procedure

Coupling of 6-(2-Fluorophenyl)-8-iodo-1-methyl-4H[1,2,4]triazolo[4,3-a] [1,4]benzodiazepine with 3,4-dihydro-4-methyl-1-(2-propynyl)-1H-1,4-benzodiazepine 2,5-dione as described in example 17 gave after chromatography and crystallization from ethyl acetate colorless crystals with m.p. 179°-182° C. The crystals of the title compound contained according to analytical and nmr-data 0.16 mol of ethyl acetate and 0.66 mol of water. The preparation of the required acetylene is described in Example 54.

Workup

  1. customgave
  2. customafter chromatography and crystallization from ethyl acetate colorless crystals with m.p. 179°-182° C

Sources & evidence

ORD record
ord-cfb40b7245f34123879309c2b8befce8
Source dataset
uspto-grants-1990_09
Patent number
US04959361

Reaction notes

Loading…