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Sodium Sulfate → HCID 9800992, 화합물

HRID 1700122
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HRID 1700122 반응식
[F:1][C:2]([F:38])([F:37])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[N:11][C:12]([CH:21]3[CH2:26][CH2:25][N:24]([C:27](OCC4C=CC=CC=4)=O)[CH2:23][CH2:22]3)=[CH:13][C:14]=2[C:15]2[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=2)[CH:6]=[CH:7][CH:8]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[F:38][C:2]([F:1])([F:37])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[N:11][C:12]([CH:21]3[CH2:22][CH2:23][N:24]([CH3:27])[CH2:25][CH2:26]3)=[CH:13][C:14]=2[C:15]2[CH:16]=[CH:17][N:18]=[CH:19][CH:20]=2)[CH:6]=[CH:7][CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 18317249HCID 18317249, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 9800992HCID 9800992, 화합물수율 53.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

Under Ar, a solution of 15 (0.73 g, 1.4 mmol) in THF (175 mL) was treated with LAH (0.37 g, 9.7 mmol). After addition, the reaction was heated at 60° C. After 2 h, the reaction was cooled to room temperature and treated with saturated Na2SO4 until a suspension results. The reaction mixture was filtered and the filtrate washed with EtOAc. The organic was washed with H2O, brine, dried, filtered and concentrated to dryness. The residue was treated with Et2O-hexanes, filtered and dried to yield 0.3 g of 16; mp 188-9° C.

후처리

  1. additionAfter addition
  2. temperaturethe reaction was cooled to room temperature
  3. customresults
  4. filtrationThe reaction mixture was filtered
  5. washthe filtrate washed with EtOAc
  6. washThe organic was washed with H2O, brine
  7. customdried
  8. filtrationfiltered
  9. concentrationconcentrated to dryness
  10. additionThe residue was treated with Et2O-hexanes
  11. filtrationfiltered
  12. customdried

출처 및 근거

ORD 기록
ord-d023c7e0d20943dd8361aaa0c4a5a851
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350744B1

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