Lithium Hydroxide → HCID 23085185, compound

HRID 916730Notes

Reaction equation

HRID 916730 reaction equation
COC(C[CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=[C:8]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[N:7]1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=O.[OH-:28].[Li+].C1[CH2:34][O:33]CC1.O>>[C:34]([CH:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=[C:8]([N:16]2[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]2)[N:7]1[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)([OH:33])=[O:28]

Participants

4

Reactant 3

HCID 3939Lithium HydroxideHCID 15262444HCID 15262444, compoundHCID 21881883Oxolane--water (1/1)

Product 1

HCID 23085185HCID 23085185, compound

Conditions

Temperature
60 °C

Procedure

The compound (6) (0.235 g, 0.645 mmol) was dissolved in 10 ml of THF/water (1:1) and a hydrate of lithium hydroxide (0.135 g, 3.23 mmol) was added thereto at a room temperature. The reaction mixture was stirred at 60° C. for 2 hours. After the reaction was completed, the pH of the reaction mixture was adjusted to 3˜4 and the reaction mixture was extracted with dichloromethane three times. An organic layer was dried with anhydrous magnesium sulfate and the solvent was removed under reduced pressure to quantitatively obtain the title compound in the form of a white crystal (7) (mp 238° C.).

Workup

  1. customat a room temperature
  2. extractionthe reaction mixture was extracted with dichloromethane three times
  3. dry with materialAn organic layer was dried with anhydrous magnesium sulfate
  4. customthe solvent was removed under reduced pressure

Sources & evidence

ORD record
ord-898ae9f4561342cdb2365efb3bfad358
Source dataset
uspto-grants-2007_09
Patent number
US07271260B2

Reaction notes

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