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Hydrochloric Acid → HCID 178494666, 화합물

HRID 1487823
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인쇄 미리보기

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HRID 1487823 반응식
[CH3:1][O:2][CH2:3][C:4]1[NH:5][C:6]([C:10]2[C:11]([CH3:21])=[CH:12][C:13]([CH3:20])=[C:14]([CH:19]=2)[C:15]([O:17]C)=[O:16])=[C:7]([CH3:9])[N:8]=1.[OH-].[Na+].Cl>CO.O>[CH3:1][O:2][CH2:3][C:4]1[NH:5][C:6]([C:10]2[C:11]([CH3:21])=[CH:12][C:13]([CH3:20])=[C:14]([CH:19]=2)[C:15]([OH:17])=[O:16])=[C:7]([CH3:9])[N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 178494667HCID 178494667, 화합물2회

생성물 1

HCID 178494666HCID 178494666, 화합물수율 98.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
40 °C

실험 절차

Into a 50-mL round-bottom flask, was placed a solution of methyl 5-(2-(methoxymethyl)-4-methyl-1H-imidazol-5-yl)-2,4-dimethylbenzoate (compound 2.1, 150 mg, 0.52 mmol) in methanol (15 mL) and H2O (5 mL). Sodium hydroxide (280 mg, 7.00 mmol) was added and the resulting solution was stirred at 40° C. for 15 h. After cooled to room temperature, the solution was adjusted to pH 5 with aqueous HCl (2 M) and the resulting mixture was concentrated under reduced pressure. The residue was dissolved in methanol (5 mL) and the solids were filtered off. The filtrate was concentrated under reduced pressure to yield the title compound as a light yellow solid (140 mg, crude), which was used in the next step without further purification.

후처리

  1. customInto a 50-mL round-bottom flask, was placed
  2. temperatureAfter cooled to room temperature
  3. concentrationthe resulting mixture was concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in methanol (5 mL)
  5. filtrationthe solids were filtered off
  6. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-acbae4e2a0354338a86694dfb2596acb
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428502B2

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