Hydrochloric Acid → HCID 15840673, 화합물

HRID 342761노트

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HRID 342761 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:29][C:30]([O:32]C)=[O:31])[CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[C:22]([CH2:23][CH2:24][CH3:25])=[C:21]2[C:16]([CH:17]=[C:18]([CH2:27][CH3:28])[C:19](=[O:26])[O:20]2)=[CH:15][CH:14]=1.[OH-].[K+].CO.Cl>CO.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:29][C:30]([OH:32])=[O:31])[CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[C:22]([CH2:23][CH2:24][CH3:25])=[C:21]2[C:16]([CH:17]=[C:18]([CH2:27][CH3:28])[C:19](=[O:26])[O:20]2)=[CH:15][CH:14]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14797Potassium HydroxideHCID 15840672HCID 15840672, 화합물

생성물 1

HCID 15840673HCID 15840673, 화합물

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

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온도
30 °C

실험 절차

To a solution of methyl 3-chloro-4-(3-ethyl-8-propyl-7-coumarinoxy)propylthio)phenylacetate (Example 3; 30 mg, 0.0613 mmol) 1.0 mL methanol:water (2:1) was added a 0.5M solution of potassium hydroxide in methanol (0.61 mL, 0.3061 mmol). The mixture was heated to 30° C. for two hours at which time the mixture was acidified to pH=3 with 1M hydrochloric acid. The aqueous solution was extracted with ethyl acetate and the combined organics were dried over magnesium sulfate, filtered, and the crude residue was purified by flash chromatography on silica gel (30% ethyl acetate/hexane/1% acetic acid) which provided the title compound

후처리

  1. extractionThe aqueous solution was extracted with ethyl acetate
  2. dry with materialthe combined organics were dried over magnesium sulfate
  3. filtrationfiltered
  4. customthe crude residue was purified by flash chromatography on silica gel (30% ethyl acetate/hexane/1% acetic acid) which

출처 및 근거

ORD 기록
ord-600c286a0c6f4008a4727f2d255022f1
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05859051

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