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2-Methyl-6-nitro-1,3-benzoxazol-4-ol → 6-Amino-2-methylbenzo[d]oxazol-4-ol

HRID 647220
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HRID 647220 반응식
[N+:1]([C:4]1[CH:13]=[C:12]([OH:14])[C:7]2[N:8]=[C:9]([CH3:11])[O:10][C:6]=2[CH:5]=1)([O-])=O.[H][H]>C1COCC1.CO.[Pd]>[NH2:1][C:4]1[CH:13]=[C:12]([OH:14])[C:7]2[N:8]=[C:9]([CH3:11])[O:10][C:6]=2[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 204858692-Methyl-6-nitro-1,3-benzoxazol-4-olHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 204858816-Amino-2-methylbenzo[d]oxazol-4-ol

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 6-nitro-4-hydroxy-2-methylbenzoxazole (5.1 g, 0.026 mole) in THF (100 ml) and methanol (50 ml) were added about 0.5 g of 10 percent palladium on carbon. The mixture was placed on the Parr-shaker apparatus and hydrogenated two hours. At this time hydrogen uptake was complete (6.3 psi, 0.079 mole). The catalyst was removed and the solvents were removed under reduced pressure. The resulting off-white solid (4.1 g, 97.0 percent) was collected and dried. TLC showed the product to be pure. A ninhydrin test for amines was positive. A silver test for hydroxylamine was negative.

후처리

  1. customwas placed on the Parr-shaker apparatus and hydrogenated two hours
  2. customThe catalyst was removed
  3. customthe solvents were removed under reduced pressure
  4. customThe resulting off-white solid (4.1 g, 97.0 percent) was collected
  5. customdried

출처 및 근거

ORD 기록
ord-e664e72264094f2dbd26e2c171168d8e
출처 데이터셋
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04407930

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