Sodium cyanoborohydride → HCID 22485666, 화합물

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[CH3:1][O:2][N:3]=[CH:4][C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[Cl:12].C([BH3-])#N.[Na+]>>[Cl:12][C:6]1[CH:7]=[C:8]([F:11])[CH:9]=[CH:10][C:5]=1[CH2:4][NH:3][O:2][CH3:1]

참가 물질

반응물 2

HCID 5003444Sodium cyanoborohydride

HCID 739889632-Chloro-4-fluoro-benzaldehyde o-methyloxime

생성물 1

HCID 22485666HCID 22485666, 화합물

실험 절차

Reduction of 2-chloro-4-fluoro-benzaldehyde O-methyloxime with sodium cyanoborohydride as described in the preparation of compound 3-B gave the title hydroxylamine as a clear oil after chromatography on silica gel (elution dichloromethane-ethyl acetate 95:5) (54% yield). 1HNMR 400 MHz (CDCl3) δ (ppm): 3.55 (3H, s, OCH3), 4.16 (2H, s, NCH2), 6.99 (1H, m, aromatic), 7.15 (1H, dd, J=2.5 Hz and J=8.6 Hz, aromatic), 7.41 (1H, dd, J=6.0 Hz and J=8.6 Hz, aromatic). The hydrochloride salt was obtained as a white solid: mp 159° C. Anal. calcd for C8H9ClFNO—HCl: C, 42.50; H, 4.46; N, 6.20. Found: C, 42.50; H, 4.36; N, 5.98.

출처 및 근거

ORD 기록: ord-7eaf068d0c25438ea52ace208495fead
출처 데이터셋: uspto-grants-2004_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06777440B2

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