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Water → HCID 9803221, 화합물

HRID 1451519
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인쇄 미리보기

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HRID 1451519 반응식
[Br:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][CH3:17])=[CH:13][CH:14]=3)[C:9]([CH:18]([CH3:25])[CH2:19][C:20]([O:22]CC)=[O:21])=[C:8]2[CH3:26])=[CH:4][CH:3]=1.[OH-].[K+].O>CCO>[Br:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][N:7]2[C:15]3[C:10](=[CH:11][C:12]([O:16][CH3:17])=[CH:13][CH:14]=3)[C:9]([CH:18]([CH3:25])[CH2:19][C:20]([OH:22])=[O:21])=[C:8]2[CH3:26])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 19974944HCID 19974944, 화합물

생성물 1

HCID 9803221HCID 9803221, 화합물수율 75%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

To a suspension of the ester from Step 4 (5.13 g, 11.5 mmol) in 50 mL of EtOH was added 8N KOH (5 mL, 40 mmol) and 5 mL water. The mixture was heated to 60° C. for 1 h, then cooled and concentrated. The residue was partitioned between 1M HCl and EtOAc. The organic phase was washed with brine, dried over MgSO4, filtered and evaporated. Crystallization from CH2Cl2/ hexanes gave 3.59 g of the title compound.

후처리

  1. temperaturecooled
  2. concentrationconcentrated
  3. customThe residue was partitioned between 1M HCl and EtOAc
  4. washThe organic phase was washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated
  8. customCrystallization from CH2Cl2/ hexanes

출처 및 근거

ORD 기록
ord-c292fa0f060a4646adbdc52b51e13241
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05604253

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