HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Toluene → HCID 178504566, compound

HRID 61864
Notes
Print preview

Reaction equation

HRID 61864 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][C:14]=1[Cl:15])[NH:11][C:10]1[C:9]([CH3:17])([CH3:16])[C:8]3[CH:18]=[C:19]([OH:22])[CH:20]=[CH:21][C:7]=3[C:6](=[O:23])[C:5]2=1.[Si:24]([O:31][CH2:32][C@H:33]1[O:37][C:36]([CH3:39])([CH3:38])[O:35][C@@H:34]1O)([C:27](C)(C)C)([CH3:26])C.[C:41]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:60]1([CH3:66])[CH:65]=CC=C[CH:61]=1.CCOC(/N=N/C(OCC)=O)=O>C1COCC1>[C:60]([C@@H:32]([O:31][SiH:24]([CH3:26])[CH3:27])[C@@H:33]1[O:37][C:36]([CH3:38])([CH3:39])[O:35][CH:34]1[CH2:41][O:22][C:19]1[CH:20]=[CH:21][C:7]2[C:6](=[O:23])[C:5]3[C:4]4[C:12](=[CH:13][C:14]([Cl:15])=[C:2]([Cl:1])[CH:3]=4)[NH:11][C:10]=3[C:9]([CH3:17])([CH3:16])[C:8]=2[CH:18]=1)([CH3:66])([CH3:65])[CH3:61]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 1140TolueneHCID 11776TriphenylphosphineHCID 5462977Diethyl azodicarboxylateHCID 66834506(4S,5R)-5-(tert-butyldimethylsilanyloxymethyl)-2,2-dimethyl-[1,3]dioxolan-4-olHCID 668345622,3-Dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

Product 1

HCID 178504566
HCID 178504566, compound
Yield 67%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
40 °C

Procedure

Under nitrogen atmosphere, to the THF (0.3 mL) solution of 2,3-dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound Y4, 12.9 mg, 0.0373 mmol), (4S,5R)-5-(tert-butyldimethylsilanyloxymethyl)-2,2-dimethyl-[1,3]dioxolan-4-ol (15.5 mg, 0.0559 mmol) and triphenylphosphine (14.7 mg, 0.0559 mmol), toluene solution (25.4 μL, 0.0559 mmol) of DEAD was added dropwise at room temperature. The reaction mixture was stirred at ambient temperature of 40° C. for 4 hr. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure, and the resulting crude product was purified by preparative TLC (Merck 60 F254, 0.5 mm) {solution for elution:hexane/ethyl acetate (3:1)} to obtain the title compound (white solid, 15.1 mg, 67%).

Workup

  1. temperatureAfter cooling to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customthe resulting crude product was purified by preparative TLC (Merck 60 F254, 0.5 mm)
  4. washfor elution

Sources & evidence

ORD record
ord-c076607dd855488094b4e339807f6902
Source dataset
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09440922B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes