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

HRID 647220
ノート
印刷プレビュー

反応式

HRID 647220 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 204858692-Methyl-6-nitro-1,3-benzoxazol-4-olHCID 178418361HCID 178418361、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e664e72264094f2dbd26e2c171168d8e
出典データセット
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04407930

反応ノート

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