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Water → (1R,2S)-(+)-cis-1-Amino-2-indanol

HRID 265745
Notes
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Reaction equation

HRID 265745 reaction equation
[C@@H:1]1(O)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][C@H:2]1[OH:10].S(=O)(=O)(O)O.O.C(#[N:20])C>>[NH2:20][C@@H:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][C@@H:2]1[OH:10]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 6342AcetonitrileHCID 247603trans-1,2-Indandiol

Product 1

HCID 2725045(1R,2S)-(+)-cis-1-Amino-2-indanol

Procedure

In 40 ml of acetonitrile, 3.0 g (20.1 mmol) of trans-(-)-1,2-indandiol (I': trans-configuration: 98.0%; cis-configuration: 2.0%; optical purity: 100% e.e.) was dissolved. At room temperature, 3.2 g (31.7 mmol) of 97% sulfuric acid was dropwise added thereto in a period of 30 minutes. After the resulting mixture was stirred at room temperature for 1 hour, the compound (I') disappeared from an HPLC. To the reaction liquid, 20 ml of water was added. Immediately thereafter, the mixture was heated and 42 ml of an acetonitrile/water azeotrope was distilled off under normal pressure. Then, the mixture was subjected to a reflux for 1.5 hours to complete the reaction. The reaction liquid was cooled to room temperature and washed twice with 10 ml of dichloromethane. Then, its pH was adjusted to 10.5 by an addition of an aqueous solution of 25% sodium hydroxide. The grayish white scaly crystal deposited thereby was filtered off under reduced pressure, washed with a small quantity of water, and then dried under reduced pressure to yield 1.77 g of cis-(-)-1-aminoindan-2-ol (V) as a primary crystal. Then, the mother liquid after the deposition of the crystal was extracted with dichloromethane and the extracted phase was concentrated to yield 0.69 g of the compound (V) as a secondary crystal.

Workup

  1. dissolutionoptical purity: 100% e.e.) was dissolved
  2. additionwas added
  3. temperatureImmediately thereafter, the mixture was heated
  4. distillation42 ml of an acetonitrile/water azeotrope was distilled off under normal pressure
  5. temperaturea reflux for 1.5 hours
  6. customthe reaction
  7. customThe reaction liquid
  8. temperaturewas cooled to room temperature
  9. washwashed twice with 10 ml of dichloromethane
  10. additionThen, its pH was adjusted to 10.5 by an addition of an aqueous solution of 25% sodium hydroxide
  11. filtrationThe grayish white scaly crystal deposited thereby was filtered off under reduced pressure
  12. washwashed with a small quantity of water
  13. customdried under reduced pressure

Sources & evidence

ORD record
ord-8e7d52d7a2204efbaac241c14b208afc
Source dataset
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05648534

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes