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

HRID 707733ノート

反応式

HRID 707733 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

反応物 2

HCID 24458Ferrous ChlorideHCID 86674241(2-Isopropyl-6-methyl-phenyl)-(1-{6-[1-(2-isopropyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-amine

生成物 1

HCID 131732194(2-Isopropyl-6-methyl-phenyl)-(1-{6-[1-(2-isopropyl-phenylimino)-ethyl]-pyridin-2-yl}-ethylidene)-amine iron (II) chloride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

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-c52eba0580b2414ba04748e8b7ae329b
出典データセット
uspto-grants-2015_11
特許番号
US09175104B2

反応ノート

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