Salicylic Acid → HCID 178454881、化合物

HRID 921986

反応式

HRID 921986 の反応式
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[OH-].[CH2:12]([P+:16]([CH2:25][CH2:26][CH2:27][CH3:28])([CH2:21][CH2:22][CH2:23][CH3:24])[CH2:17][CH2:18][CH2:19][CH3:20])[CH2:13][CH2:14][CH3:15]>CC(C)=O>[C:1]([O-:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[CH2:25]([P+:16]([CH2:12][CH2:13][CH2:14][CH3:15])([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:21][CH2:22][CH2:23][CH3:24])[CH2:26][CH2:27][CH3:28].[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4]

参加物

4

反応物 2

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

生成物 1

HCID 178454881HCID 178454881、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Salicylic acid (5-20 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.) with stirring for 24 hrs. 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.74 (dd, J1=7.7 Hz, J2=1.9 Hz, 1H), 7.32 (dt, J1=7.6 Hz, J2=1.8 Hz, 1H), 6.8 (m, 2H), 2.20 (m, 4 H), 1.41 (m, 8 H), 0.9 (t, J=7.1 Hz, 6 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.1. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=171.9(s), 163.1(s), 131.1 (d), 129.8(d), 120.6 (s), 115.7 (d), 115.6 (d), 23.3 (d, J=16.4 Hz), 22.6 (d, J=4.8 Hz), 17.3 (d, J=47.3 Hz), 13.2 (s).

後処理

  1. customThe solvent was evaporated
  2. customthe remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.)
  3. stirringwith stirring for 24 hrs

出典と根拠

ORDレコード
ord-79fdd7867a444a6eb52723b3abf9171b
出典データセット
uspto-grants-2016_03
特許番号
US09278134B2

関連ノート

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