Hydrochloric Acid → HCID 68519468, 화합물

HRID 386741노트

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HRID 386741 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:25]([F:28])([F:27])[F:26])[O:13][N:12]=[C:11]([C:14]3[CH:23]=[CH:22][C:17]([C:18](OC)=[O:19])=[C:16]([CH3:24])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([C:25]([F:27])([F:26])[F:28])[O:13][N:12]=[C:11]([C:14]3[CH:23]=[CH:22][C:17]([CH2:18][OH:19])=[C:16]([CH3:24])[CH:15]=3)[CH2:10]2)[CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 21226445Aluminium lithium hydrideHCID 59563501Methyl 4-(5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazol-3-yl)-2-methylbenzoate

생성물 1

HCID 68519468HCID 68519468, 화합물수율 96.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of methyl 4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazol-3-yl]-2-methylbenzoate (1.0 g) in tetrahydrofuran (30 mL) was added dropwise to a solution of lithium aluminum hydride (0.1 g) in tetrahydrofuran (50 mL) under ice cooling, and, after finishing the addition, the mixture was stirred for one hour at room temperature. The reaction solution was poured onto ice, and then 2N hydrochloric acid (30 mL) was added by portions. The mixture was extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a crude product of {4-[5-(3,5-dichlorophenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazol-3-yl]-2-methylphenyl}methanol (0.9 g).

후처리

  1. additionthe addition
  2. additionThe reaction solution was poured onto ice
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-fec39e2be1c34416b0683bac28386e97
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372867B2

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