Potassium Hydroxide → 3-Fluoro-4-(oxetan-3-yloxy)benzoic acid

HRID 2204189

반응식

HRID 2204189 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[O:12][CH:13]1[CH2:16][O:15][CH2:14]1)[C:5]([O:7]C)=[O:6].[OH-].[K+]>CO>[F:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[O:12][CH:13]1[CH2:14][O:15][CH2:16]1)[C:5]([OH:7])=[O:6]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 58550731Methyl 3-fluoro-4-(oxetan-3-yloxy)benzoate

생성물 1

HCID 566044493-Fluoro-4-(oxetan-3-yloxy)benzoic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Crude methyl 3-fluoro-4-(oxetan-3-yloxy)benzoate from Step 1, MeOH (1 mL), and KOH (4.0 mL of 3.0 M, 12 mmol) were combined and the mixture was allowed to stir for 3 h at rt. The mixture was extracted with EtOAc and the organic layer was discarded. The aqueous layer was then treated with 1N HCl and the pH was adjusted to pH 3. The aqueous layer was extracted with EtOAc (3×) and the combined organic layers were dried over sodium sulfate and the solvent was removed. The crude acid was used without further purification. ESI-MS m/z calc. 212.1, found 213.0 (M+1)+; Retention time: 1.65 minutes (4 min run).

후처리

  1. extractionThe mixture was extracted with EtOAc
  2. additionThe aqueous layer was then treated with 1N HCl
  3. extractionThe aqueous layer was extracted with EtOAc (3×)
  4. dry with materialthe combined organic layers were dried over sodium sulfate
  5. customthe solvent was removed
  6. customThe crude acid was used without further purification
  7. customRetention time: 1.65 minutes (4 min run)

출처 및 근거

ORD 기록
ord-06ccacd31d2a4bbca48841caec0e30b4
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365588B2

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