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Hydrochloric Acid → HCID 49847246, 화합물

HRID 1930104
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인쇄 미리보기

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HRID 1930104 반응식
[OH-].[K+].[C:3]([C:6]1[N:11]=[C:10]([C:12]2[CH:17]=[C:16]([F:18])[C:15]([C:19]3[CH:24]=[CH:23][C:22]([CH2:25][C:26]([O:28]C)=[O:27])=[CH:21][C:20]=3[Cl:30])=[C:14]([F:31])[CH:13]=2)[C:9]([CH3:32])=[N:8][C:7]=1[CH3:33])(=[O:5])[NH2:4].Cl>C(O)(C)(C)C>[C:3]([C:6]1[N:11]=[C:10]([C:12]2[CH:17]=[C:16]([F:18])[C:15]([C:19]3[CH:24]=[CH:23][C:22]([CH2:25][C:26]([OH:28])=[O:27])=[CH:21][C:20]=3[Cl:30])=[C:14]([F:31])[CH:13]=2)[C:9]([CH3:32])=[N:8][C:7]=1[CH3:33])(=[O:5])[NH2:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 59627738HCID 59627738, 화합물2회

생성물 1

HCID 49847246HCID 49847246, 화합물수율 77.2%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

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온도
50 °C

실험 절차

Powdered potassium hydroxide (111 mg, 1.98 mmol) was added in one portion to methyl 2-(4′-(6-carbamoyl-3,5-dimethylpyrazin-2-yl)-2-chloro-2′,6′-difluorobiphenyl-4-yl)acetate (Intermediate 2-1; 295 mg, 0.66 mmol) in tert-butanol (10 mL) at 50° C. The resulting solution was stirred at 50° C. for 45 minutes, 2M HCl (2 mL) was added and the mixture was evaporated to remove the organic solvent. The suspension was collected by filtration, washed with water (50 mL) and air dried to afford 2-(4′-(6-carbamoyl-3,5-dimethylpyrazin-2-yl)-2-chloro-2′,6′-difluorobiphenyl-4-yl)acetic acid (220 mg, 77%) as a cream solid.

후처리

  1. customthe mixture was evaporated
  2. customto remove the organic solvent
  3. filtrationThe suspension was collected by filtration
  4. washwashed with water (50 mL) and air
  5. customdried

출처 및 근거

ORD 기록
ord-d96db8fc0c8246079f16bd0a86311a71
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188092B2

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