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Hydroxyamine hydrochloride → HCID 58531385, 화합물

HRID 1889694
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반응식

HRID 1889694 반응식
[F:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][C:7]2[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=2)[CH:10]=O)=[CH:4][CH:3]=1.Cl.[NH2:18][OH:19]>CO>[F:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][C:7]2[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=2)/[CH:10]=[N:18]/[OH:19])=[CH:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 3085320Benzaldehyde, 3-(4-fluorophenoxy)-

생성물 1

HCID 58531385HCID 58531385, 화합물수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a mixture of 3-(4-fluorophenoxy)benzaldehyde (3.0 g, 13.8 mmol, 1.0 eq) in methanol was added hydroxylamine hydrochloride (1.06 g, 15.2 mmol, 1.1 eq). The reaction mixture was stirred at ambient temperature for 12 h, before being concentrated in vacuo. The residue was taken in ethyl acetate and washed with water. The organic layer was dried with anhydrous Na2SO4 and concentrated to obtain the desired product (3 g, 94%). 1H NMR (400 MHz, DMSO-d6) δ 8.12 (s, 1H), 7.42-7.38 (t, 1H), 7.32-7.31 (d, 1H), 7.27-7.23 (t, 2H), 7.16 (s, 1H), 7.13-7.10 (m, 2H), 7.01-6.99 (m, 1H). MS (ESI): 232.2 (M+H)+.

후처리

  1. concentrationbefore being concentrated in vacuo
  2. washwashed with water
  3. dry with materialThe organic layer was dried with anhydrous Na2SO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-80eb8cbac60c407988afafe7fc59d49c
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501992B2

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