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O-Methylhydroxylamine hydrochloride → HCID 76614995, 화합물

HRID 2103036
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HRID 2103036 반응식
[CH2:1]([C:3]1[C:15]([OH:16])=[C:14]([CH3:17])[C:13]([CH3:18])=[C:12]2[C:4]=1[C:5](=O)[CH2:6][C:7]1([O:11]2)[CH2:10][CH2:9][CH2:8]1)[CH3:2].Cl.[CH3:21][O:22][NH2:23]>N1C=CC=CC=1>[CH3:21][O:22][N:23]=[C:5]1[C:4]2[C:12](=[C:13]([CH3:18])[C:14]([CH3:17])=[C:15]([OH:16])[C:3]=2[CH2:1][CH3:2])[O:11][C:7]2([CH2:10][CH2:9][CH2:8]2)[CH2:6]1
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참가 물질

4

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 69053766HCID 69053766, 화합물

생성물 1

HCID 76614995HCID 76614995, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 5-ethyl-6-hydroxy-7,8-dimethylspiro[chromene-2,1′-cyclobutan]-4(3H)-one (0.51 g) in 9 mL of pyridine was added methoxyamine hydrochloride (0.82 g). The reaction mixture was allowed to stir at room temperature overnight. The mixture was extracted with ethyl acetate, washed with 1N HCl, and concentrated in vacuo to give 5-ethyl-6-hydroxy-7,8-dimethylspiro[chromene-2,1′-cyclobutan]-4(3H)-one O-methyloxime, 1H-NMR (300 MHz, CDCl3) δ=4.58 (s, 1H, 4.01 (s, 3H), 3.05 (m, 2H), 3.02 (s, 2H), 2.20 (s, 3H), 2.17 (s, 3H), 2.10-1.60 (m, 6H), 1.24 (t, 3H) ppm. 13C-NMR (75 MHz, CDCl3) δ=151.0, 147.4, 146.3, 125.8, 124.6, 124.3, 115.3, 76.9, 61.9, 33.9, 33.4, 21.2, 13.6, 12.7, 12.3, 12.1 ppm. MS: (m/z)=290.1 (M+H+).

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. washwashed with 1N HCl
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-44e2fca42b834b19bb89c832dbf6b384
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576094B2

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