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Water → 3-[(3,5-Di-tert-butyl-4-hydroxyphenyl)sulfanyl]propanoic acid

HRID 359736
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HRID 359736 반응식
[CH3:1][C:2]([C:5]1[CH:6]=[C:7]([S:16][CH2:17][CH2:18][C:19]([O:21]C)=[O:20])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])[CH3:3].O.[OH-].[Li+].O>CO>[CH3:15][C:12]([C:9]1[CH:8]=[C:7]([S:16][CH2:17][CH2:18][C:19]([OH:21])=[O:20])[CH:6]=[C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])[C:10]=1[OH:11])([CH3:13])[CH3:14]
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참가 물질

5

반응물 3

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 13531084HCID 13531084, 화합물

생성물 1

HCID 150352573-[(3,5-Di-tert-butyl-4-hydroxyphenyl)sulfanyl]propanoic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 3-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]propanoate (1.0 g, 3 mmole) was added to a clear solution of lithium hydroxide hydrate (0.64 g, 15 mmole) in methanol (15 ml). Water was added until the solution became cloudy and the mixture was then stirred overnight. The mixture was concentrated to about 10 ml and acidified with cold (5° ) 10% hydrochloric acid. The resultant precipitate was collected by filtration, washed with water, and air dried Recrystallization from cyclohexane gave the title compound, m.p. 108°-110°.

후처리

  1. concentrationThe mixture was concentrated to about 10 ml
  2. customacidified with cold (5° ) 10% hydrochloric acid
  3. filtrationThe resultant precipitate was collected by filtration
  4. washwashed with water, and air
  5. customdried
  6. customRecrystallization from cyclohexane

출처 및 근거

ORD 기록
ord-5ef6444245da46d38210c19b03166982
출처 데이터셋
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05002967

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