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HCID 15045041, 화합물 → 3-(9H-Fluoren-9-yl)propanoic acid

HRID 2259275
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반응식

HRID 2259275 반응식
[CH:1]1[C:13]2[CH:12]([CH2:14][CH2:15][CH:16]3[O:20]CC[O:17]3)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1>CC(C)=O.CC(C)=O.OS(O)(=O)=O.O=[Cr](=O)=O>[CH:1]1[C:13]2[CH:12]([CH2:14][CH2:15][C:16]([OH:20])=[O:17])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 15045041HCID 15045041, 화합물

생성물 1

HCID 135008763-(9H-Fluoren-9-yl)propanoic acid

시약·촉매·용매 2

HCID 180Acetone용매HCID 131709961Jones' reagent용매

실험 절차

3-(9-Fluorenyl)propionic acid was prepared from 2-(9-fluorenyl)ethyl-1,3-dioxolane (50.0 g, 187 mmol) which was dissolved in 20 ml of acetone and 450 ml of Jones' reagent (64 g chromic acid and 64 ml of sulfuric acid in 400 ml of water). After the reaction was complete, the acetone was evaporated, the residue taken into ethyl acetate, washed with water, and organic layer extracted with 1N sodium hydroxide which was acidified with 10% HCl to yield a tan precipitate. FTIR 1954, 1913, 1707, 1429, 1316, 1257, 1208, 948, 933, 735 cm-1. 1H NMR (300 MHz, DMSO-dis) δ 1.84 (t, 2H, J=7.5 Hz), 2.21 (m, 2H), 4.03 (t, 2H, J=5.5 Hz), 7.28-7.38 (m, 4H), 7.56 (d, 2H, J=7.0 Hz), 7.84 (d, 2H, J=7.0 Hz).

후처리

  1. customthe acetone was evaporated
  2. washwashed with water, and organic layer
  3. extractionextracted with 1N sodium hydroxide which
  4. customto yield a tan precipitate

출처 및 근거

ORD 기록
ord-84ef42d6a0ff4e66bd7725248f6d1b14
출처 데이터셋
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05472973

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