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Hydrochloric Acid → HCID 67672163, 화합물

HRID 1417551
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인쇄 미리보기

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HRID 1417551 반응식
C[O:2][C:3]([C@H:5]1[CH2:30][CH2:29][C@:7]2([O:11][CH2:10][C@H:9]([C:12]3[CH:17]=[C:16]([N:18]4[CH:22]=[CH:21][N:20]=[C:19]4[C:23]([F:26])([F:25])[F:24])[CH:15]=[CH:14][C:13]=3[O:27][CH3:28])[CH2:8]2)[C@@H:6]1[C:31]1[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=1)=[O:4].[OH-].[Na+].Cl>C(O)C.O>[F:37][C:34]1[CH:35]=[CH:36][C:31]([C@H:6]2[C@@H:5]([C:3]([OH:4])=[O:2])[CH2:30][CH2:29][C@@:7]32[O:11][CH2:10][C@H:9]([C:12]2[CH:17]=[C:16]([N:18]4[CH:22]=[CH:21][N:20]=[C:19]4[C:23]([F:26])([F:25])[F:24])[CH:15]=[CH:14][C:13]=2[O:27][CH3:28])[CH2:8]3)=[CH:32][CH:33]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 56974282HCID 56974282, 화합물

생성물 1

HCID 67672163HCID 67672163, 화합물수율 103%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
0 °C

실험 절차

To an ice cold solution of 40 mg (0.077 mmol) (3S,5R,6S,7S)-6-(4-fluorophenyl)-3-(2-methoxy-5-(2-trifluoromethylimidazol-1-yl)phenyl)-1-oxaspiro[4.4]nonane-7-carboxylic acid methyl ester (from Example 70) in 1.0 mL of ethanol and 0.20 mL of water was added 0.050 mL of 2.5N aqueous NaOH. The mixture was stirred at 0° C., then warmed slowly to RT overnight. After neutralizing with 0.065 mL of 2N aqueous HCl, the mixture was partitioned between 25 mL of ethyl acetate and 25 mL of brine. The layers were separated and the organic layer was dried over sodium sulfate and evaporated to give 40 mg of title compound as a colorless syrup. Mass spectrum (NH3/CI): m/z=505.0 (M+1).

후처리

  1. temperaturewarmed slowly to RT overnight
  2. customthe mixture was partitioned between 25 mL of ethyl acetate and 25 mL of brine
  3. customThe layers were separated
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-734052d1bf674d6f8fb9fffa361c78b1
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05877191

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