Hydrogen Bromide → CHROMAN-8-OL

HRID 581071노트

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HRID 581071 반응식
C[O:2][C:3]1[C:12]2[O:11][CH2:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.Br.C1(O)C=CC=CC=1>C(O)(=O)C>[OH:2][C:3]1[C:12]2[O:11][CH2:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 996PhenolHCID 13758736HCID 13758736, 화합물

생성물 1

HCID 19033254CHROMAN-8-OL

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

The compound obtained in Step C (1 g; 6.09 mmol) is dissolved in glacial acetic acid (10.2 ml) and then hydrobromic acid (48% solution in water) (3.7 eq.; 47 mmol; 2.54 ml) is added dropwise. The phenol is fully deprotected after 5 hours' reflux. After removal of the solvent under reduced pressure, the dry residue is taken up in aqueous medium and then neutralised with a saturated sodium hydrogen carbonate solution to a pH of 8. Extraction with ethyl acetate yields an orange oil after drying and concentration. After purification of the latter over a silica column. AcOEt/PE (3:7), the oil is yellow in colour.

후처리

  1. temperature' reflux
  2. customAfter removal of the solvent under reduced pressure
  3. extractionExtraction with ethyl acetate
  4. customyields an orange oil
  5. customafter drying
  6. concentrationconcentration
  7. customAfter purification of the latter over a silica column

출처 및 근거

ORD 기록
ord-899b9f5b4ad14e8990d08d5c80c8e64b
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919814

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