Triethylamine → HCID 178439034、化合物

HRID 1441210ノート

反応式

HRID 1441210 の反応式
[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[N:13]1[CH2:17][C:16](=[NH:18])[N:15]([C:19]2[C:24]([CH:25]([CH3:27])[CH3:26])=[CH:23][CH:22]=[CH:21][C:20]=2[CH:28]([CH3:30])[CH3:29])[CH2:14]1)([CH3:3])[CH3:2].[Cl-:31].[Cl-].[Cl-].[CH:34]1([Ti+3:39])[CH:38]=[CH:37][CH:36]=[CH:35]1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl-:31].[Cl-:31].[CH:34]1([Ti+2:39])[CH:38]=[CH:37][CH:36]=[CH:35]1.[CH:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH:10]([CH3:12])[CH3:11])[C:5]=1[N:13]1[CH2:17][C:16](=[NH:18])[N:15]([C:19]2[C:20]([CH:28]([CH3:30])[CH3:29])=[CH:21][CH:22]=[CH:23][C:24]=2[CH:25]([CH3:27])[CH3:26])[CH2:14]1)([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 866152461,3-Bis(2,6-diisopropylphenyl)-iminoimidazolineHCID 178478623HCID 178478623、化合物

生成物 1

HCID 178439034HCID 178439034、化合物収率 46%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
4 °C

実験手順

To a suspension of 1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline (2.03 g, 5.0 mmol) and cyclopentadienyltitanium trichloride (1.10 g, 5.0 mmol) in toluene (30 mL) was added triethylamine (0.8 mL, 5,7 mmol) at ambient temperature. After stiriring for 1 hour, the thick yellow-orange suspension was diluted with toluene (50 mL) and ligroin (120 mL). The suspension was heated to reflux and filtered hot. Cooling to approx. 4° C. afforded yellow crystals, which were filtered and washed with cold ligroin to give 1.34 g (46% yield) of NMR pure 1,3-bis(2,6-diisopropylphenyl)-iminoimidazoline cyclopentadienyl titanium dichloride.

後処理

  1. temperatureThe suspension was heated
  2. temperatureto reflux
  3. filtrationfiltered hot
  4. customafforded yellow crystals, which
  5. filtrationwere filtered
  6. washwashed with cold ligroin

出典と根拠

ORDレコード
ord-da3d6ae50f12465285d9389e6cc6deb2
出典データセット
uspto-grants-2010_02
特許番号
US07655592B2

反応ノート

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