Hydrochloric Acid → HCID 15840671, 화합물

HRID 342757노트

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HRID 342757 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]([C:17]([CH2:27][CH3:28])=[CH:18][C:19](=[O:26])[O:20]2)=[CH:15][CH:14]=1.[OH-].[K+].Cl>CO.O.CO>[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]([C:17]([CH2:27][CH3:28])=[CH:18][C:19](=[O:26])[O:20]2)=[CH:15][CH:14]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 15840670HCID 15840670, 화합물

생성물 1

HCID 15840671HCID 15840671, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 22242641Methanol--water (1/1)용매

반응 조건

온도
40 °C

실험 절차

To a solution of methyl 3-chloro-4-(3-(4-ethyl-8-propyl-7-coumarinoxy)propylthio)phenylacetate (Example 1; 82 mg, 0.1677 mmol) in 1.2 mL methanol:water (1:1) was added a 0.5M solution of potassium hydroxide in methanol. The mixture was heated to 40° C. for two hours at which time the mixture was acidified to pH=3 with 1M aqueous 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-a30c04ac4b43426089b48b5e595810af
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05859051

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