Aluminum ethylate → HCID 178515945、化合物

HRID 1470063ノート

反応式

HRID 1470063 の反応式
[CH:1]1[CH:20]=[CH:19][C:17](=[O:18])/[C:3](=[CH:4]\[NH:5][CH2:6][CH2:7][NH:8]/[CH:9]=[C:10]2\[C:11]([CH:13]=[CH:14][CH:15]=[CH:16]\2)=[O:12])/[CH:2]=1.[O-]CC.[O-]CC.[O-]CC.[Al+3]>C1(C)C=CC=CC=1>[CH:15]1[CH:14]=[CH:13][C:11](=[O:12])/[C:10](=[CH:9]/[NH:8][CH2:7][CH2:6][NH:5]/[CH:4]=[C:3]2/[CH:2]=[CH:1][CH:20]=[CH:19][C:17]/2=[O:18])/[CH:16]=1

参加物

4

反応物 2

HCID 11153Aluminum ethylateHCID 178515944HCID 178515944、化合物

生成物 1

HCID 178515945HCID 178515945、化合物収率 114.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Salen ligand (C0) (1.0 g, 3.9 mmol) and aluminium triethoxide (1.2 g, 7.4 mmol) were dissolved in dry toluene (25 mL). The reaction mixture was refluxed for 4 hours after which the toluene was evaporated and the resulting yellow residue taken up in dichloromethane and washed with water (3×100 mL) and saturated brine (100 mL). After evaporation of the organic phase, a light yellow powder was obtained which was washed with diethyl ether (ca. 50 mL) and dried to give salen complex (C1) (1.2 g, 49%). 1H NMR 3.87 (8H, s, 2×CH2CH2), 6.7-6.9 (8H, m, 8×HAr), 7.1-7.3 (8H, m, 8×HAr), 8.29 (4H, s, 4×CHN). 13C NMR 60.14, 65.09, 117.36, 119.00, 131.81, 132.74, 161.46, 166.85. m/z (ESI) Found: 603.1775 C32H25N4O5Al2 (MH+), Requires 603.1769.

後処理

  1. customwas evaporated
  2. washwashed with water (3×100 mL) and saturated brine (100 mL)
  3. customAfter evaporation of the organic phase
  4. customa light yellow powder was obtained which
  5. washwas washed with diethyl ether (ca. 50 mL)
  6. customdried

出典と根拠

ORDレコード
ord-5a1a717f4b834325a63db0c94b9a7361
出典データセット
uspto-grants-2015_04
特許番号
US09006425B2

反応ノート

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