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Water → HCID 19928725、化合物

HRID 1885211
ノート
印刷プレビュー

反応式

HRID 1885211 の反応式
[CH3:1][NH:2][CH:3]([C:6]([CH3:19])([OH:18])[CH2:7][CH2:8][CH2:9][CH:10]([CH3:17])[CH2:11][CH2:12][CH2:13][CH:14]([CH3:16])[CH3:15])[CH2:4][OH:5].N1C=CC=CC=1.Cl.[C:27](Cl)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[N:30][CH:29]=1.O>ClC(Cl)C>[CH3:1][N:2]([CH:3]([C:6]([OH:18])([CH3:19])[CH2:7][CH2:8][CH2:9][CH:10]([CH3:17])[CH2:11][CH2:12][CH2:13][CH:14]([CH3:15])[CH3:16])[CH2:4][OH:5])[C:27](=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[N:30][CH:29]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 199287142-(N-Methylamino)-3,7,11-trimethyl-1,3-dodecanediol

生成物 1

HCID 19928725HCID 19928725、化合物収率 93%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane
溶媒

反応条件

温度
-30 °C

実験手順

In 100 ml of dichloroethane were dissolved 10 g of 2-(methylamino)-3,7,11-trimethyl-1,3-dodecanediol and 8.7 g of pyridine and the solution was cooled to -30° C. To this solution was added 7.2 g of nicotinoyl chloride hydrochloride gradually and the mixture was stirred at room temperature for 3 hours. After the reaction was completed, the reaction mixture was poured into water and extracted with dichloroethane. The organic layer was washed with aqueous sodium hydrogen carbonate and after drying over anhydrous magnesium sulfate, the solvent was distilled off. Finally, the residue was subjected to silica gel column chromatography (elution with ethanol) to give 12.0 g of N-methyl-N-(1,3-dihydroxy-3,7,11-trimethyldodecan-2-yl)nicotinamide [Compound (66)]. Yield 93%.

後処理

  1. extractionextracted with dichloroethane
  2. washThe organic layer was washed with aqueous sodium hydrogen carbonate
  3. dry with materialafter drying over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. washFinally, the residue was subjected to silica gel column chromatography (elution with ethanol)

出典と根拠

ORDレコード
ord-476268ff3e9f45abacfff9fc6722308b
出典データセット
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05143921

反応ノート

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