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Potassium Carbonate → 9-(8-aza-bicyclo[3.2.1]oct-3-ylidene)-5-methoxy-9H-xanthene-3-carboxylic acid diethylamide

HRID 733397
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HRID 733397 반응식
[CH2:1]([N:3]([CH2:36][CH3:37])[C:4]([C:6]1[CH:7]=[CH:8][C:9]2[C:10](=[C:22]3[CH2:28][CH:27]4[N:29](C(=O)C(F)(F)F)[CH:24]([CH2:25][CH2:26]4)[CH2:23]3)[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[C:15]([O:20][CH3:21])[CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>CO>[CH2:36]([N:3]([CH2:1][CH3:2])[C:4]([C:6]1[CH:7]=[CH:8][C:9]2[C:10](=[C:22]3[CH2:23][CH:24]4[NH:29][CH:27]([CH2:26][CH2:25]4)[CH2:28]3)[C:11]3[C:16]([O:17][C:18]=2[CH:19]=1)=[C:15]([O:20][CH3:21])[CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:37]
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 578392625-Methoxy-9-[8-(2,2,2-trifluoro-acetyl)-8-aza-bicyclo[3.2.1]oct-3-ylidene]-9H-xanthene-3-carboxylic acid diethylamide2회

생성물 1

HCID 111775769-(8-aza-bicyclo[3.2.1]oct-3-ylidene)-5-methoxy-9H-xanthene-3-carboxylic acid diethylamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5-methoxy-9-[8-(2,2,2-trifluoro-acetyl)-8-aza-bicyclo[3.2.1]-oct-3ylidene]-9H-xanthene-3-carboxylic acid diethylamide, 5c (3.2g, 6.22 mmol) and potassium carbonate (1.89 g, 13.7 mmol) in methanol (50 mL) was stirred at rt overnight. The mixture was evaporated, and partitioned between methylene chloride (100 mL) and water (100 mL). The organic layer was separated, dried over sodium sulfate, filtered, and evaporated, yielding 2.72 g of 9-(8-aza-bicyclo[3.2.1]oct-3-ylidene)-5-methoxy-9H-xanthene-3-carboxylic acid diethylamide, 6c. MS m/z=419.0 (MH+).

후처리

  1. customThe mixture was evaporated
  2. custompartitioned between methylene chloride (100 mL) and water (100 mL)
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-a14745aed8454bb4bbbffd096d72d657
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07589104B2

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