Methanol → Potassium 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate

HRID 1269379노트

반응식

HRID 1269379 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:27]=[CH:26][C:21]([C:22]([O:24]C)=[O:23])=[CH:20][CH:19]=3)[CH:14]=2)=[CH:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH3:5].CO.[OH-].[K+:31]>O1CCCC1>[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]([O-:24])=[O:23])=[CH:26][CH:27]=3)[CH:14]=2)=[CH:11][CH:12]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[K+:31]

참가 물질

5

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 10737571Methyl 4-(5-(4-(pentyloxy)phenyl)isoxazol-3-yl)benzoate

생성물 1

HCID 23670213Potassium 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
55 °C

실험 절차

Methyl 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate (16.4 kg), tetrahydrofuran (164 L), methanol (25 L) and 19% aqueous potassium hydroxide (25 L) were put into a 1500 L glass-lined reaction chamber, heated to 50 to 60° C., and stirred for 2 hours. Tetrahydrofuran (328 L) was added to this reaction mixture for 30 minutes to 1 hour. The mixture was then cooled to 35 to 40° C. and stirred further for 1 hour. The product was isolated by a centrifugal separator and washed with tetrahydrofuran (164 L) to obtain rough potassium 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate (which was used in the next step in a wet state).

후처리

  1. temperatureThe mixture was then cooled to 35 to 40° C.
  2. stirringstirred further for 1 hour
  3. customThe product was isolated by a centrifugal separator
  4. washwashed with tetrahydrofuran (164 L)

출처 및 근거

ORD 기록
ord-2868fd4f2bbb40589b1767e39b0df54f
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199248B2

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