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Lithium aluminum hydride → HCID 20031070, 화합물

HRID 232146
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HRID 232146 반응식
[Li+].[AlH4-].[F:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:14]3[CH2:15][CH2:16][CH2:17][C:13]=3[C:12]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][C:23](O)=[O:24])=[N:11]2)=[CH:6][CH:5]=1>C1COCC1>[F:3][C:4]1[CH:5]=[CH:6][C:7]([N:10]2[C:14]3[CH2:15][CH2:16][CH2:17][C:13]=3[C:12]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][OH:24])=[N:11]2)=[CH:8][CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 28112Lithium aluminum hydrideHCID 14576185HCID 14576185, 화합물

생성물 1

HCID 20031070HCID 20031070, 화합물수율 44.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

Lithium tetrahydridoaluminate (0.345 g, 9.1 mmol) in THF (75 ml) was treated with the compound of Example 31 (1.0 g, 3.1 mmol) and the mixture was heated at 60° C. for 2 hours. Excess reagent was quenched, the mixture filtered and the combined filtrate and ethyl acetate washes were evaporated to a colorless oil (0.76 g). Polar impurities were removed on silica gel (40 g) with 1:1 ethyl acetate-Skelly B eluent to provide title compound (0.42 g) as an oil.

후처리

  1. customExcess reagent was quenched
  2. filtrationthe mixture filtered
  3. customthe combined filtrate and ethyl acetate washes were evaporated to a colorless oil (0.76 g)
  4. customPolar impurities were removed on silica gel (40 g) with 1:1 ethyl acetate-Skelly B eluent

출처 및 근거

ORD 기록
ord-5dbc443e95534e3c9b94a293ff1a7720
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851425

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