Water → HCID 54136706, 화합물

HRID 1681625노트

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HRID 1681625 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14](OC)=[O:15])=[C:12]([CH3:18])[N:11]=[C:10]([CH:19]([CH3:21])[CH3:20])[C:9]=2[C:22](OCC)=[O:23])=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[K+]>O1CCCC1>[OH:23][CH2:22][C:9]1[C:10]([CH:19]([CH3:21])[CH3:20])=[N:11][C:12]([CH3:18])=[C:13]([CH2:14][OH:15])[C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 10155368HCID 10155368, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 54136706HCID 54136706, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

20.7 g (57.7 mmol) of the compound from Example 26 dissolved in 50 ml of absolute tetrahydrofuran are slowly added dropwise under nitrogen to a suspension of 6 g (158 mmol) of lithium aluminum hydride in 200 ml of absolute tetrahydrofuran at 60° C. The mixture is heated to reflux for 1 h, cooled to 0° C. and 18 ml of water are cautiously added. 6 ml of 10% strength potassium hydroxide solution are added to the mixture, it is filtered off from the precipitate with suction and the residue is boiled twice using 250 ml of ether each time. The combined mother liquors are dried over magnesium sulphate and concentrated in vacuo. The residue is stirred with petroleum ether, filtered off with suction and dried in a desiccator.

후처리

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 1 h
  3. filtrationis filtered off from the precipitate with suction
  4. dry with materialThe combined mother liquors are dried over magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. filtrationfiltered off with suction
  7. customdried in a desiccator

출처 및 근거

ORD 기록
ord-e70025bd65f04124a989705ee0466317
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05173495

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