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Lithium hydroxide, monohydrate → 2-Chloro-3-(1-cyanocyclobutyl)benzoic acid

HRID 1800617
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HRID 1800617 반응식
[Cl:1][C:2]1[C:11]([C:12]2([C:16]#[N:17])[CH2:15][CH2:14][CH2:13]2)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].O.[OH-].[Li+]>O1CCCC1.CO.O>[Cl:1][C:2]1[C:11]([C:12]2([C:16]#[N:17])[CH2:15][CH2:14][CH2:13]2)=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]
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참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 68416730HCID 68416730, 화합물

생성물 1

HCID 684190472-Chloro-3-(1-cyanocyclobutyl)benzoic acid수율 65%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Methyl 2-chloro-3-(1-cyanocyclobutyl)benzoate (710 mg, 2.84 mmol) was dissolved in a mixed solvent of tetrahydrofuran (9 mL)/methanol (3 mL)/water (3 mL), lithium hydroxide monohydrate (192 mg, 4.56 mmol) was added, and the mixture was stirred at room temperature for 19 hr. The reaction mixture was concentrated under reduced pressure, and 1N hydrochloric acid (5 mL) was added dropwise to the residue. The precipitate was collected by filtration, and washed with water to give the title compound (435 mg, 65%) as a white powder.

후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and 1N hydrochloric acid (5 mL)
  3. additionwas added dropwise to the residue
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water

출처 및 근거

ORD 기록
ord-3811154acefa47d1a90e5f4413e1aa8a
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344135B2

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