Triethylamine → N-(3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine

HRID 448878

반응식

HRID 448878 반응식
[CH2:1]1[CH2:11][C:9](=O)[C:8]2[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:2]1.Cl.[NH2:13][OH:14].C(N(CC)CC)C>CO>[C:9]1(=[N:13][OH:14])[C:8]2[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:2][CH2:1][CH2:11]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 107241-TetraloneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 76876N-(3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine수율 108.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of α-tetralone (10 g, 68.5 mmol) in anhydrous MeOH (175 mL), hydroxylamine hydrochloride (7.6 g, 109.6 mmol) and triethylamine (15.3 mL, 109.6 mmol) were added. The mixture was stirred at room temperature for 16 hrs, followed by removal of the solvent in vacuo. The residue was dissolved in DCM, washed with water and brine, dried (Na2SO4), filtered and concentrated in vacuo to yield crude 3,4-dihydro-2H-naphthalen-1-one oxime (12 g). MS [M+H]+: 162.1; tR=2.03 min. (method 1)

후처리

  1. customfollowed by removal of the solvent in vacuo
  2. dissolutionThe residue was dissolved in DCM
  3. washwashed with water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e6abb06940f34a21842540b7f830e82c
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481738B2

연결된 노트

불러오는 중…