Sodium Hydroxide → HCID 59561114, 화합물

HRID 1918435노트

반응식

HRID 1918435 반응식
[CH3:1][C:2]1[C:14]2[C:13](=O)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[CH3:16])[C:6]=2[CH:5]=[C:4]([CH3:17])[CH:3]=1.I.[OH-].[Na+]>C(O)(=O)CC.O>[CH3:1][C:2]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[CH3:16])[C:6]=2[CH:5]=[C:4]([CH3:17])[CH:3]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 24841Hydrogen iodideHCID 57909153HCID 57909153, 화합물2회

생성물 1

HCID 59561114HCID 59561114, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1032Propionic Acid용매

실험 절차

1,3,8-Trimethylfluoren-9-one (53) was reduced according to the general procedure of Carruthers et al. (W. Carruthers, D. Whitmarsh, J. Chem. Soc. Perkin Trans, I 1973, 1511). 1,3,8-Trimethylfluoren-9-one (53) (2.74 g, 12.3 mmol) was dissolved in propionic acid (235 ml). Red phosphorus (3.0 g) and concentrated HI (40 ml) were added and the reaction mixture was refluxed for 24 h. Quantitative conversion was shown by TLC. The reaction mixture was diluted with water (250 ml), neutralized with NaOH and extracted with Et2O (4×125 ml). The combined organic layers were washed with brine (2×125 ml), dried over MgSO4, filtered and the volatiles removed in vacuo to afford 2.56 g (quant.) 54 as a white solid.

후처리

  1. temperaturethe reaction mixture was refluxed for 24 h
  2. extractionextracted with Et2O (4×125 ml)
  3. washThe combined organic layers were washed with brine (2×125 ml)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe volatiles removed in vacuo

출처 및 근거

ORD 기록
ord-3df40ec1fed24af089656ebffef515d4
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618328B2

반응 노트

불러오는 중…