HCID 86755658, compound → HCID 86755659, compound

HRID 1871995Notes

Reaction equation

HRID 1871995 reaction equation
[CH2:1]([C:3]1[CH:50]=[CH:49][C:6]2[CH:7]([C:17]3[C:18]([S:47]C)=[N:19][C:20](=[O:46])[N:21]([C:23]4[CH:28]=[CH:27][N:26]=[C:25]([N:29]([CH3:45])[CH2:30][C:31]([NH:33][C:34]5[S:35][CH:36]=[C:37]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])[N:38]=5)=[O:32])[N:24]=4)[CH:22]=3)[C:8]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:9]=3[CH:10]=[CH:11][C:5]=2[CH:4]=1)[CH3:2]>N1C=CC=CC=1.C(N(CC)CC)C>[CH2:1]([C:3]1[CH:50]=[CH:49][C:6]2[CH:7]([C:17]3[C:18](=[S:47])[NH:19][C:20](=[O:46])[N:21]([C:23]4[CH:28]=[CH:27][N:26]=[C:25]([N:29]([CH3:45])[CH2:30][C:31]([NH:33][C:34]5[S:35][CH:36]=[C:37]([CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])[N:38]=5)=[O:32])[N:24]=4)[CH:22]=3)[C:8]3[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][C:9]=3[CH:10]=[CH:11][C:5]=2[CH:4]=1)[CH3:2]

Participants

4

Reactant 1

HCID 86755658HCID 86755658, compound

Product 1

HCID 86755659HCID 86755659, compound

Reagents, catalysts & solvents 2

HCID 1049PyridineSolventHCID 8471TriethylamineSolvent

Procedure

The product from step (v) (0.61 g) was dissolved in dry pyridine (20 ml) and triethylamine (1.0 ml). Hydrogen sulphide gas was slowly bubbled through the solution for 15 minutes. The solvents were evaporated under reduced pressure and the residue azeotroped twice with toluene. The residue was purified by chromatography eluting with ethyl acetate in toluene. Yield 0.41 g.

Workup

  1. customHydrogen sulphide gas was slowly bubbled through the solution for 15 minutes
  2. customThe solvents were evaporated under reduced pressure
  3. customthe residue azeotroped twice with toluene
  4. customThe residue was purified by chromatography
  5. washeluting with ethyl acetate in toluene

Sources & evidence

ORD record
ord-9b192823e3be4dffaac6af1fb1edc8a0
Source dataset
uspto-grants-2000_08
Patent number
US06107297

Reaction notes

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