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Potassium sodium tartarate → HCID 67056312, 화합물

HRID 714645
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HRID 714645 반응식
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][N:18]=1)[C:12](OC)=[O:13].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[Na+]>C1COCC1>[F:19][C:2]([F:1])([F:20])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([CH2:12][OH:13])[CH:16]=[CH:17][N:18]=1
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참가 물질

5

반응물 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 67396524HCID 67396524, 화합물

생성물 1

HCID 67056312HCID 67056312, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

432 mg (1.54 mmol) of the compound from Example 58A were dissolved in 10 ml of THF, and 1.08 ml (1.08 mmol) of a 1 M solution of lithium aluminum hydride in THF were added at −10° C. After the addition had ended, the mixture was stirred at RT for 2 h. For work-up, 4 ml of a saturated sodium potassium tartrate solution were added at RT, and the mixture was extracted with 15 ml of ethyl acetate. The organic phase was washed once with 10 ml of saturated sodium potassium tartrate solution, dried over magnesium sulfate, filtered and concentrated under reduced pressure. This gave 497 mg (>100% of theory) of the target compound which were reacted further without any further purification.

후처리

  1. additionAfter the addition
  2. extractionthe mixture was extracted with 15 ml of ethyl acetate
  3. washThe organic phase was washed once with 10 ml of saturated sodium potassium tartrate solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThis gave 497 mg (>100% of theory) of the target compound which were reacted further without any further purification

출처 및 근거

ORD 기록
ord-415161255ab148c5b224d675d6e329b8
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187466B2

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