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Ammonia → 4-Amino-6-benzyloxy-2,2-dimethylchroman

HRID 618818
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HRID 618818 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][C:14]([CH3:20])([CH3:19])[CH2:13][C:12]2=[N:21]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N>C1COCC1.CO.[Ni]>[NH2:21][CH:12]1[C:11]2[C:16](=[CH:17][CH:18]=[C:9]([O:8][CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH:10]=2)[O:15][C:14]([CH3:20])([CH3:19])[CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 867545186-Benzyloxy-2,2-dimethylchroman-4-one oxime

생성물 1

HCID 212645054-Amino-6-benzyloxy-2,2-dimethylchroman

시약·촉매·용매 2

HCID 935Nickel촉매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

30 g of 6-benzyloxy-2,2-dimethylchroman-4-one oxime were dissolved in 900 ml of THF/methanol (1:1), treated with 25 ml of aqueous ammonia and hydrogenated in a shaking duck using Raney Ni. The catalyst was then filtered off with suction, the filtrate was concentrated in vacuo, the residue was dissolved in EA, dried and concentrated, and the residue was crystallized using petroleum ether, 22.9 g, m.p. 86-88° C.

후처리

  1. filtrationThe catalyst was then filtered off with suction
  2. concentrationthe filtrate was concentrated in vacuo
  3. dissolutionthe residue was dissolved in EA
  4. customdried
  5. concentrationconcentrated
  6. customthe residue was crystallized

출처 및 근거

ORD 기록
ord-42c78d6848124d6db8a0b782dd2c9e92
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05955607

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