HCID 67119435, 화합물 → HCID 67119420, 화합물

HRID 384833노트

반응식

HRID 384833 반응식
[CH3:1][C:2]1[C:13]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=2)=[CH:12][C:5]([C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[O:7])=[C:4]([N+:26]([O-])=O)[CH:3]=1>[C].[Pd].CO>[NH2:26][C:4]1[CH:3]=[C:2]([CH3:1])[C:13]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:23])([F:24])[F:25])=[CH:17][CH:16]=2)=[CH:12][C:5]=1[C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[O:7]

참가 물질

4

반응물 1

HCID 67119435HCID 67119435, 화합물

생성물 1

HCID 67119420HCID 67119420, 화합물수율 95.1%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

An 80% methanol (225 g), 50 g of isopropyl 4-methyl-2-nitro-5-(4-(trifluoromethoxy)phenoxy)benzoate, and 2.5 g of a 5% palladium carbon were charged into a 500-ml stainless steel autoclave equipped with a stirring device and a thermometer, and a reaction was allowed to proceed under a hydrogen pressure of 0.5 MPa at 30° C. for 6 hr. After the replacement of the air in the autoclave with nitrogen, the reaction solution was filtered using 220 ml of methanol to remove the catalyst. The methanol solution thus obtained was concentrated under the reduced pressure, and 208 ml of water was added to the residue. The precipitated solid was collected by filtration and was dried to give isopropyl 2-amino-4-methyl-5-(4-(trifluoromethoxy)phenoxy)benzoate (43.96 g, yield: 95%).

후처리

  1. customequipped with a stirring device
  2. customat 30° C.
  3. customfor 6 hr
  4. filtrationAfter the replacement of the air in the autoclave with nitrogen, the reaction solution was filtered
  5. customto remove the catalyst
  6. customThe methanol solution thus obtained
  7. concentrationwas concentrated under the reduced pressure, and 208 ml of water
  8. additionwas added to the residue
  9. filtrationThe precipitated solid was collected by filtration
  10. customwas dried

출처 및 근거

ORD 기록
ord-49bf7e32d61f4c0bbe843588ff6d2726
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367833B2

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