Methylamine → 2-[(2-bromophenyl)-hydrazono]-N-methyl-2-cyanoacetamide

HRID 2375587노트

반응식

HRID 2375587 반응식
C(O[C:4](=[O:17])[C:5](=[N:8][NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[Br:16])[C:6]#[N:7])C.[CH3:18][NH2:19]>O>[Br:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[NH:9][N:8]=[C:5]([C:6]#[N:7])[C:4]([NH:19][CH3:18])=[O:17]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 4084583[(2-Bromophenyl)-hydrazono]-cyanoacetic acid ethyl ester

생성물 1

HCID 866130992-[(2-bromophenyl)-hydrazono]-N-methyl-2-cyanoacetamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

[(2-Bromophenyl)-hydrazono]-cyanoacetic acid ethyl ester (15.28 g, 51.60 mmol) was dissolved in 40% methylamine in water (67.5 mL) and stirred at room temperature overnight. The reaction mixture was concentrated to dryness, slurried in diethyl ether, and filtered. After drying under high vacuum at 40° C., the title compound was obtained as a yellow solid (11.16 g, 77%). 1H NMR (300.132 MHz, CDCl3) δ 7.68 (dd, J=8.2, 1.4 Hz, 1H), 7.54 (dd, J=8.1, 1.3 Hz, 1H), 7.35 (t, J=7.9 Hz, 1H), 7.01 (td, J=7.7, 1.5 Hz, 1H), 6.29 (s, 1H), 2.98 (d, J=4.9 Hz, 3H). MS APCI, m/z=281/283 (M+H). HPLC 4.08 min.

후처리

  1. concentrationThe reaction mixture was concentrated to dryness
  2. filtrationfiltered
  3. customAfter drying under high vacuum at 40° C.

출처 및 근거

ORD 기록
ord-a82ec8a6d9694b508ca413e223cdc74f
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07465795B2

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