Ferrous Chloride → (2-Isopropyl-6-methyl-phenyl)-(1-{6-[1-(2-isopropyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-amine iron (II) chloride

HRID 1406601ノート

反応式

HRID 1406601 の反応式
[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:5]=1[N:11]=[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20](=[N:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[CH:29]([CH3:31])[CH3:30])[CH3:21])[N:15]=1)[CH3:13])([CH3:3])[CH3:2].[Fe:32]([Cl:34])[Cl:33]>C1COCC1>[Fe:32]([Cl:34])[Cl:33].[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:5]=1[N:11]=[C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20](=[N:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[CH:29]([CH3:31])[CH3:30])[CH3:21])[N:15]=1)[CH3:13])([CH3:3])[CH3:2]

参加物

4

実験手順

2.42 g (0.0059 mol) of (2-Isopropyl-6-methyl-phenyl)-(1-{6-[1-(2-isopropyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-amine 16 (2.42 g, 0.0059 mol) was added in one portion to the suspension of 0.71 g (0.0056 mol) of iron (II) chloride in 40 ml of THF at ambient temperature under nitrogen glove box. The reaction mixture was stirred for 12 h. The resultant blue solid was filtered and washed by 50 ml of pentanes three times and dried under 1-mm vacuum overnight. The yield of (2-isopropyl-6-methyl-phenyl)-(1-{6-[1-(2-isopropyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-amine iron (II) chloride 17 was 2.29 g (76%).

後処理

  1. filtrationThe resultant blue solid was filtered
  2. washwashed by 50 ml of pentanes three times
  3. customdried under 1-mm vacuum overnight

出典と根拠

ORDレコード
ord-45d44a9a226e49cbad5c2a40369fbac3
出典データセット
uspto-grants-2014_12
特許番号
US08916664B2

反応ノート

読み込み中…