Sodium Bicarbonate → 2-Amino-5-chloro-2'-hydroxybenzophenone

HRID 1797

반응식

HRID 1797 반응식
[NH2:1][C:2]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12]C)=[O:5].C(=O)(O)[O-].[Na+]>Br>[NH2:1][C:2]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[OH:12])=[O:5]

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 12325893(2-Amino-5-chlorophenyl)(2-methoxyphenyl)methanone

생성물 1

HCID 5264882-Amino-5-chloro-2'-hydroxybenzophenone수율 93.4%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

A mixture of 2.15 g of 2-amino-5-chloro-2'-methoxybenzophenone and 20 ml of 47% hydrogen bromide was heated for 1 hour under reflux. The solution was rendered neutral with sodium bicarbonate, and subjected to extraction with 100 ml of ethyl acetate. The extract solution was washed with water and dried over anhydrous magnesium sulfate; the solvent was then distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1) to yield 1.9 g of 2-amino-5-chloro-2'-hydroxybenzophenone as needles, m.p. 51° to 52° C.

후처리

  1. temperaturewas heated for 1 hour
  2. temperatureunder reflux
  3. extractionsubjected to extraction with 100 ml of ethyl acetate
  4. washThe extract solution was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was then distilled off under reduced pressure
  7. customThe residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1)

출처 및 근거

ORD 기록
ord-b12632ff90da4c7fbf9aead0149dd2e8
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726306

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