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Acetic Acid → HCID 22630262, 화합물

HRID 2416352
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인쇄 미리보기

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HRID 2416352 반응식
[C:1]([O:4][C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:8][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].C(O)(=O)C.C(OC(=O)C)(=O)C.[Br:29]Br>O>[Br:29][C:11]1[CH:12]=[CH:13][C:14]2[C:15]3[C:7](=[CH:6][C:5]([O:4][C:1](=[O:3])[CH3:2])=[CH:17][CH:16]=3)[CH2:8][C:9]=2[CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 7918Acetic AnhydrideHCID 24408BromineHCID 2470609h-Fluoren-2-yl acetate

생성물 1

HCID 22630262HCID 22630262, 화합물수율 72.9%

시약·촉매·용매 1

HCID 962Water용매

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온도
65 °C

실험 절차

2-Acetoxyfluorene (70 g) was added to a mixture of acetic acid (330 mL) and acetic anhydride (110 mL) and heated up to 65° C. to obtain a homogeneous solution. Bromine (125 g) was dropwise added thereto in 40 minutes and stirred for further one hour. The reaction solution was poured into water (1 L) to obtain deposited crystals by filtration under reduced pressure. The dried crystals were ecrystallized from a mixed solution of ethanol (400 mL) and ethyl acetate (300 mL) to obtain colorless needle-shaped 2-bromo-7-acetoxyfluorene (69 g). The melting point of this compound was 130° C.

후처리

  1. customto obtain a homogeneous solution
  2. customto obtain
  3. filtrationby filtration under reduced pressure

출처 및 근거

ORD 기록
ord-15806a48208d480295fad10b3d68f6ab
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06824709B2

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