Hydrochloric Acid → 4-(5-(4-(Pentyloxy)phenyl)-3-isoxazolyl)benzoic acid

HRID 1269380노트

반응식

HRID 1269380 반응식
[CH2:1]([O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[O:17][N:16]=[C:15]([C:18]3[CH:26]=[CH:25][C:21]([C:22]([O-:24])=[O:23])=[CH:20][CH:19]=3)[CH:14]=2)=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[K+].O1CCCC1.Cl>O>[CH2:1]([O:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[O:17][N:16]=[C:15]([C:18]3[CH:19]=[CH:20][C:21]([C:22]([OH:24])=[O:23])=[CH:25][CH:26]=3)[CH:14]=2)=[CH:11][CH:12]=1)[CH2:2][CH2:3][CH2:4][CH3:5]

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid2회HCID 8028TetrahydrofuranHCID 23670213Potassium 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate

생성물 1

HCID 99752244-(5-(4-(Pentyloxy)phenyl)-3-isoxazolyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

The pure potassium 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate obtained in Example 2, tetrahydrofuran (131 L) and water (131 L) were put into a 1000 L glass-lined reaction chamber, heated to 45 to 55° C., and 1N hydrochloric acid (82 L) was added to this reaction mixture for 20 or more minutes. Furthermore, water (607 L) was added to the reaction mixture for 30 or more minutes at the same temperature. This reaction mixture was cooled to 25 to 35° C. and its pH was adjusted to 3 or less with 6N hydrochloric acid. The product was isolated by a centrifugal separator and washed with water (164 L) and acetone (82 L) and dried by a vacuum drier to obtain pure 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoic acid (14.9 kg).

후처리

  1. temperatureThis reaction mixture was cooled to 25 to 35° C.
  2. customThe product was isolated by a centrifugal separator
  3. washwashed with water (164 L) and acetone (82 L)
  4. customdried by a vacuum drier

출처 및 근거

ORD 기록
ord-11001e7f5e1b46db8c3a5bce8366f06f
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199248B2

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