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Water → HCID 67807745, 화합물

HRID 1609559
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HRID 1609559 반응식
[CH:1]1([C:4]2[N:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[C:7](C(OCC)=O)=[C:6]([C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=3)[C:5]=2[CH2:25][O:26][CH3:27])[CH2:3][CH2:2]1.[OH2:28].[C:29]1(C)C=CC=CC=1>O1CCCC1>[CH:1]1([C:4]2[N:9]([CH3:29])[CH:8]([CH:10]([CH3:12])[CH3:11])[C:7]([OH:28])=[C:6]([C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=3)[C:5]=2[CH2:25][O:26][CH3:27])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 1140TolueneHCID 20081807HCID 20081807, 화합물

생성물 1

HCID 67807745HCID 67807745, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

44.3 ml (15 mmol) of a 3.5 molar solution of sodium bis-(2-methoxyethoxy)-dihydroaluminate in toluene are added under nitrogen to a solution of 1.9 g (5 mmol) of the compound from Example 83 in 50 ml of dry tetrahydrofuran and the mixture is stirred for 2 hours at room temperature and 1 hour under reflux. After cooling to 0° C., 50 ml of water are cautiously added dropwise and the mixture is extracted several times with ethyl acetate. The ethyl acetate phases are combined, washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated in vacuo.

후처리

  1. temperatureunder reflux
  2. temperatureAfter cooling to 0° C.
  3. extractionthe mixture is extracted several times with ethyl acetate
  4. washwashed with saturated sodium chloride solution
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ca0ca926de774e4ebd7a95b9cb23a131
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05401746

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