Aluminium lithium hydride → HCID 20031090, 화합물

HRID 232149노트

반응식

HRID 232149 반응식
C([O:3][C:4]([C:6]1[C:10]2[CH2:11][CH2:12][CH2:13][C:9]=2[N:8]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:7]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH2:14]([N:8]1[C:9]2[CH2:13][CH2:12][CH2:11][C:10]=2[C:6]([CH2:4][OH:3])=[N:7]1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 54375111HCID 54375111, 화합물

생성물 1

HCID 20031090HCID 20031090, 화합물수율 1,065.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 1-benzyl-1,4,5,6-tetrahydro-3-cyclopentapyrazole carboxylic acid ethyl ester (6.0 g, 2.22 mmol) in THF (125 ml) was treated with lithium aluminum hydride (1.73 g, 44.4 mmol) and reacted at ambient temperature for 3.5 hours. Excess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml). The mixture was diluted with ethyl acetate and filtered. The filtrate was washed with 5% brine solutions, dried, and evaporated to provide the title compound (5.40 g) as an oil.

후처리

  1. customreacted at ambient temperature for 3.5 hours
  2. customExcess reagent was quenched with 10% aqueous THF (18 ml), 15% sodium hydroxide (5.4 ml) and water (5.4 ml)
  3. additionThe mixture was diluted with ethyl acetate
  4. filtrationfiltered
  5. washThe filtrate was washed with 5% brine solutions
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-ba1834a51b864f498493990d2345a5a1
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851425

반응 노트

불러오는 중…