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Benzyl Alcohol → HCID 86663454, compound

HRID 446555
Notes
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Reaction equation

HRID 446555 reaction equation
[C:1]([O:5][C:6]([N:8]([CH3:27])[CH2:9][CH2:10][CH2:11][N:12]1[CH2:21][CH2:20][C:19]2[C:14](=[CH:15][CH:16]=[C:17](C(OC)=O)[CH:18]=2)[C:13]1=[O:26])=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+].Cl.[N-]=[N+]=[N-].P([O-])(OC1C=CC=CC=1)(OC1C=CC=CC=1)=O.C(N(CC)CC)C.C(O)C1C=CC=CC=1.C(OC(N(C)CCCN1CCC2C(=CC=[C:82]([NH:87][C:88](=[O:97])[O:89][CH2:90][C:91]3[CH:96]=[CH:95][CH:94]=[CH:93][CH:92]=3)C=2)C1=O)=O)(C)(C)C.CI.[H-].[Na+]>O1CCCC1.CO.CN(C)C=O.C(OCC)(=O)C.O>[C:1]([O:5][C:6]([N:8]([CH3:27])[CH2:9][CH2:10][CH2:11][N:12]1[CH2:21][CH2:20][C:19]2[C:14](=[CH:15][CH:16]=[C:17]([CH2:82][NH:87][C:88](=[O:97])[O:89][CH2:90][C:91]3[CH:96]=[CH:95][CH:94]=[CH:93][CH:92]=3)[CH:18]=2)[C:13]1=[O:26])=[O:7])([CH3:4])([CH3:2])[CH3:3]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

15

Reactant 9

HCID 244Benzyl AlcoholHCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 21964642Diphenylphosphate azide
HCID 66671432
Methyl 2-{3-([tert-butoxycarbonyl)(methyl)amino]propyl}-1-oxo-1,2,3,4-tetrahydroisoquinoline-6-carboxylate
HCID 86663455Benzyl (2-{3-([tert-butoxycarbonyl)(methyl)amino]propyl}-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl)carbamate

Product 1

HCID 86663454HCID 86663454, compoundYield 88%

Reagents, catalysts & solvents 5

HCID 887MethanolSolventHCID 962WaterSolventHCID 6228DimethylformamideSolventHCID 8028TetrahydrofuranSolventHCID 8857Ethyl AcetateSolvent2×

Conditions

Temperature
60 °C

Procedure

The compound (535 mg, 1.41 mmol) obtained in Example 61c was dissolved in a mixed solvent (6 mL) of tetrahydrofuran and methanol (1:1), a 1 N aqueous sodium hydroxide solution (1 mL) was added, and the mixture was stirred at 60° C. for 5 hours. After the reaction was completed, a 1 N aqueous hydrochloric acid solution (10 mL) was added to the reaction mixture under ice cooling, and ethyl acetate was further added to separate the layers. The resulting organic layer was separated, washed with saturated sodium chloride solution, and then dried with anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was dissolved in 1,4-dioxane (6 mL), diphenyl phosphate azide (0.238 mL, 1.10 mmol), triethylamine (0.154 mL, 1.10 mmol) and benzyl alcohol (0.228 mL, 2.21 mmol) were added under ice cooling, and the mixture was stirred at 100° C. under a nitrogen atmosphere for 16 hours. After the reaction was completed, the solvent was evaporated under reduced pressure, the resulting crude benzyl (2-{3-([tert-butoxycarbonyl)(methyl)amino]propyl}-1-oxo-1,2,3,4-tetrahydroisoquinolin-6-yl)carbamate (354 mg, 0.757 mmol) was dissolved in N,N-dimethylformamide (7 mL), methyl iodide (0.236 mL, 3.79 mmol) and 55% sodium hydride (40 mg, 0.909 mmol) were added under ice cooling, and the mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour. After the reaction was completed, water was added to the reaction mixture under ice cooling, and ethyl acetate was further added to separate the layers. The resulting organic layer was separated, washed with saturated sodium chloride solution, and then dried with anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate, 1:5, v/v) to give the title compound (320 mg; yield, 88%) as a colorless oily substance.

Workup

  1. customto separate the layers
  2. customThe resulting organic layer was separated
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried with anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. dissolutionThe resulting residue was dissolved in 1,4-dioxane (6 mL)
  7. stirringthe mixture was stirred at 100° C. under a nitrogen atmosphere for 16 hours
  8. customthe solvent was evaporated under reduced pressure
  9. stirringthe mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour
  10. customto separate the layers
  11. customThe resulting organic layer was separated
  12. washwashed with saturated sodium chloride solution
  13. dry with materialdried with anhydrous sodium sulfate
  14. customthe solvent was evaporated under reduced pressure
  15. customThe residue was purified by silica gel column chromatography (hexane

Sources & evidence

ORD record
ord-94e0ba7de3e140d1a2bf01148ff5f58a
Source dataset
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08476253B2

Reaction notes

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