Aluminum ethylate → HCID 178515945, 화합물

HRID 1470063노트

반응식

HRID 1470063 반응식
[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

참가 물질

4

반응물 2

HCID 11153Aluminum ethylateHCID 178515944HCID 178515944, 화합물

생성물 1

HCID 178515945HCID 178515945, 화합물수율 114.7%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a1a717f4b834325a63db0c94b9a7361
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006425B2

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