Lithium Hydroxide → 3-(5-p-Tolyl-isoxazol-3-yl)-benzoic acid

HRID 2113908노트

반응식

HRID 2113908 반응식
C[O:2][C:3](=[O:22])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[CH:14]=[C:13]([C:15]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=3)[O:12][N:11]=2)[CH:5]=1.[OH-].[Li+]>O1CCOCC1>[C:18]1([CH3:21])[CH:17]=[CH:16][C:15]([C:13]2[O:12][N:11]=[C:10]([C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:3]([OH:22])=[O:2])[CH:14]=2)=[CH:20][CH:19]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 57907091Methyl 3-(5-p-tolylisoxazol-3-yl)benzoate

생성물 1

HCID 579071533-(5-p-Tolyl-isoxazol-3-yl)-benzoic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

In a 25 ml round flask, 330 mg (1.13 mmol) of 3-[5-p-tolyl-isoxazol-3-yl]-benzoic acid methyl ester is dissolved in 10 ml of dioxane and subsequently 1.69 ml of aqueous lithium hydroxide (1M, 1.69 mmol, 1.5 eq.) are added and the resulting solution stirred for 20 h at room temperature. Then, the dioxane is removed in vacuo, 10 ml of water are added and the pH adjusted to 2 with hydrochloric acid (1M). The precipitate is filtered and dried to yield the title compound as a white solid. Mass spectrum: m/z (M−H)+: 278.2

후처리

  1. customThen, the dioxane is removed in vacuo, 10 ml of water
  2. additionare added
  3. filtrationThe precipitate is filtered
  4. customdried

출처 및 근거

ORD 기록
ord-591d636e6d83455a96a5761dba17be02
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432293B2

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