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Hydrochloric Acid → 4-Methyl-2-sulfanylbenzoic acid

HRID 539951
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HRID 539951 반응식
CN(C)C([S:5][C:6]1[CH:15]=[C:14]([CH3:16])[CH:13]=[CH:12][C:7]=1[C:8]([O:10]C)=[O:9])=O.Cl>[OH-].[Na+]>[CH3:16][C:14]1[CH:13]=[CH:12][C:7]([C:8]([OH:10])=[O:9])=[C:6]([SH:5])[CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21761355Methyl 2-[(dimethylcarbamoyl)sulfanyl]-4-methylbenzoate

생성물 1

HCID 200954184-Methyl-2-sulfanylbenzoic acid

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
0 °C

실험 절차

A round bottle flask containing a mixture of methyl 2-[(dimethylcarbamoyl)sulfanyl]-4-methylbenzoate (50 g, 197.6 mmol) and an aqueous solution of sodium hydroxide (120 mL, 4 N) was vacuumed and backfilled with nitrogen 3 times. After being refluxed for 2 hours, the resulting mixture was cooled to 0° C. and acidified with an aqueous solution of hydrochloric acid (45 mL, 6 N). The formed precipitate was collected by filtration, and then dissolved in ethyl acetate (500 mL). The solution was dried over anhydrous sodium sulfate, and concentrated in vacuo to afford 4-methyl-2-sulfanylbenzoic acid as a light yellow solid.

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후처리

  1. additionA round bottle flask containing
  2. temperatureAfter being refluxed for 2 hours
  3. filtrationThe formed precipitate was collected by filtration
  4. dissolutiondissolved in ethyl acetate (500 mL)
  5. dry with materialThe solution was dried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5870ec31c9344498bc9543a92cbe5025
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871756B2

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