Ethanol → HCID 13293066, 화합물

HRID 904817노트

반응식

HRID 904817 반응식
[C:1]([NH:9][CH:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]1=[O:20])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(O)C>C1COCC1>[CH2:1]([NH:9][C@@H:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C@H:11]1[OH:20])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 13293063N-(1-Oxo-1,2,3,4-tetrahydronaphthalen-2-yl)benzamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 13293066HCID 13293066, 화합물수율 897.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 2-benzamido-3,4-dihydronaphthalen-1(2H)-one (3.0 g, 1.1 mmole) in THF (150 ml) was added dropwise to a suspension of LiAlH4 (2.0 g) in THF (50 ml). The reaction was heated at reflux for 2 hr and then cooled to room temperature. Enough ethanol was added to destroy excess LiAlH4 followed by 150 ml of Rochell's salt solution (20%). The resulting mixture was extracted with ethyl acetate, the ethyl acetate layer was washed with brine and dried over Na2SO4. Evaporation of the solvent afforded 2.5 g (88%) of the product, m.p. 110°-114° C. After recrystallization from cyclohexane it had m.p. 112°-115° C.

후처리

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 2 hr
  3. customto destroy excess LiAlH4
  4. extractionThe resulting mixture was extracted with ethyl acetate
  5. washthe ethyl acetate layer was washed with brine
  6. dry with materialdried over Na2SO4
  7. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-f43725a652944e8fa58691821f871460
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420480

반응 노트

불러오는 중…