Dichloromethane → HCID 86583898, compound

HRID 637211Notes

Reaction equation

HRID 637211 reaction equation
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[N:19]([N:20]([CH3:24])[C:21](=[O:23])[CH3:22])[C:18]3[CH:25]=[CH:26][CH:27]=[CH:28][C:17]=3[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.ClCCl.[IH:32]>C(OCC)C>[IH:32].[CH3:24][N:20]([N:19]1[C:18]2[CH:25]=[CH:26][CH:27]=[CH:28][C:17]=2[N:16]=[C:15]1[N:11]1[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]1)[C:21](=[O:23])[CH3:22]

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 24841Hydrogen iodideHCID 18464583HCID 18464583, compound

Product 1

HCID 86583898HCID 86583898, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

Combine 1-(t-butoxycarbonyl)-4-(1-(N-methylacetamido)-1H-benzimidazol-2-yl)[1,4]diazepane (0.18 g, 0.48 mmol) and dichloromethane (10 mL). Add hydriodic acid (0.17 mL, 57%, 0.95 mmol) and warm to 40° C. After 3 hours, cool to ambient temperature and evaporate in vacuo to give a residue. Combine the residue and diethyl ether with stirring to give a solid. Collect the solid by filtration to give, after drying, the title compound.

Workup

  1. customevaporate in vacuo
  2. customto give a residue
  3. customto give a solid
  4. customCollect the solid
  5. filtrationby filtration
  6. customto give
  7. customafter drying

Sources & evidence

ORD record
ord-fb769ebfd7ea4f54990ced11fb10d67c
Source dataset
uspto-grants-2001_02
Patent number
US06194406B1

Reaction notes

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