Salicylic Acid → HCID 178473643、化合物

HRID 921992

反応式

HRID 921992 の反応式
[C:1]([OH:6])(=[O:5])[CH:2]([CH3:4])[OH:3].[C:7]([OH:16])(=[O:15])[C:8]1[C:9](=[CH:11][CH:12]=[CH:13][CH:14]=1)[OH:10].[OH-].[CH2:18]([P+:22]([CH2:31][CH2:32][CH2:33][CH3:34])([CH2:27][CH2:28][CH2:29][CH3:30])[CH2:23][CH2:24][CH2:25][CH3:26])[CH2:19][CH2:20][CH3:21]>CC(C)=O>[C:7]([O-:16])(=[O:15])[C:8]1[C:9](=[CH:11][CH:12]=[CH:13][CH:14]=1)[OH:10].[CH2:31]([P+:22]([CH2:18][CH2:19][CH2:20][CH3:21])([CH2:23][CH2:24][CH2:25][CH3:26])[CH2:27][CH2:28][CH2:29][CH3:30])[CH2:32][CH2:33][CH3:34].[C:1]([OH:6])(=[O:5])[CH:2]([CH3:4])[OH:3]

参加物

5

反応物 3

HCID 338Salicylic AcidHCID 612Lactic AcidHCID 84487Phosphonium, tetrabutyl-, hydroxide (1:1)

生成物 1

HCID 178473643HCID 178473643、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Lactic acid (0.4504 g, 5 mmol), salicylic acid (0.6909 g, 5 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone and stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried at 0.01 mbar with stirring for 24 hrs. The desired compound is isolated as a colourless liquid; 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.63 (dd, J1=7.6 Hz, J2=1.9 Hz), 7.11 (m, 1H), 6.58 (m, 3H), 4.03 (q, J=6.9 Hz, 1H), 2.17 (m, 8H), 1.42 (m, 16 H), 1.23 (d, 7.0 Hz, 3H), 0.90 (t, J=7.3 Hz, 12 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.0. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=176.3, 171.1, 163.0, 131.2, 129.9, 120.5, 117.8, 115.767.3, 23.4 (d, J=15.8 Hz), 22.6 (d, J=4.3 Hz), 20.5, 17.3 (d, J=47.7 Hz), 13.3 (s).

後処理

  1. customThe solvent was evaporated
  2. customthe remaining viscous liquid was dried at 0.01 mbar
  3. stirringwith stirring for 24 hrs

出典と根拠

ORDレコード
ord-0260974b33fc4dec97a88a0eb2af9a0b
出典データセット
uspto-grants-2016_03
特許番号
US09278134B2

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