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

HRID 2375587ノート

反応式

HRID 2375587 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

[(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.

後処理

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

出典と根拠

ORDレコード
ord-a82ec8a6d9694b508ca413e223cdc74f
出典データセット
uspto-grants-2008_12
特許番号
US07465795B2

反応ノート

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