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

Water → 2-Bromo-5,6-dichloro-indan-1-ol

HRID 574636
Notes
Print preview

Reaction equation

HRID 574636 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[CH2:7][CH:6]=[CH:5]2.[Br:12]C1C=C(F)C=C2C=1CC=C2.[OH2:23]>CS(C)=O>[Br:12][CH:6]1[CH2:5][C:4]2[C:8](=[CH:9][C:10]([Cl:11])=[C:2]([Cl:1])[CH:3]=2)[CH:7]1[OH:23]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 962WaterHCID 199195275,6-dichloro-1H-indeneHCID 684621937-bromo-5-fluoro-1H-indene

Product 1

HCID 894445282-Bromo-5,6-dichloro-indan-1-ol

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Conditions

Temperature
25 °C

Procedure

According to Scheme 2, step IV: To a solution of 5,6-dichloro-1H-indene (5f) (1.28 g, 6.92 mmol), which was obtained according to Scheme 2 by following a reaction sequence according to synthesis of (5a), in dimethylsulfoxide (6.5 ml) and water (0.16 ml) N-bromosuccinimide (2.44 g, 13.7 mmol) was added at 10° C. and the mixture was stirred at 25° C. for 1 h. The mixture was poured on water, stirred for 30 min and the solid material was filtered off. The crude product was purified by silica gel chromatography (eluting with 0 to 50% ethyl acetate in heptane) to give 1.46 g of 2-bromo-5,6-dichloro-indan-1-ol which was immediately dissolved in tetrahydrofuran (35 ml). Finely powdered NaOH (1.37 g, 34.2 mmol) was added and the mixture was stirred at 25° C. for 2 h. The mixture was filtered through a short pad of celite and washed with a small amount of ethyl acetate. The filtrate was evaporated to dryness to give 1 g of racemic(1aS,6aR)-3,4-Dichloro-6,6a-dihydro-1aH-1-oxa-cyclopropa[a]indene (6f), which was used in the next step without purification.

Workup

  1. additionThe mixture was poured on water
  2. stirringstirred for 30 min
  3. filtrationthe solid material was filtered off
  4. customThe crude product was purified by silica gel chromatography (eluting with 0 to 50% ethyl acetate in heptane)

Sources & evidence

ORD record
ord-aca68ae87b474e27b646d1bba1623170
Source dataset
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09034897B2

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes