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Water → HCID 131731068、化合物

HRID 1192453
ノート
印刷プレビュー

反応式

HRID 1192453 の反応式
[CH2:1]([OH:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[CH2:10](N(C(C)C)C(C)C)C.[CH2:19]([Si:37](C)(Cl)Cl)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36].O>C1(C)C=CC=CC=1>[CH3:10][CH:20]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH3:36])[CH2:19][SiH:37]1[O:9][CH2:1][C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4]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 5146Salicyl AlcoholHCID 78835Silane, dichloromethyloctadecyl-HCID 81531Diisopropylethylamine

生成物 1

HCID 131731068HCID 131731068、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
45 °C

実験手順

In a 1 l four-neck flask with stirrer, reflux condenser and dropping funnel, 31.7 g of salicyl alcohol (0.25 mol) and 66.7 g (0.52 mol) of dried N-ethyldiisopropylamine were suspended under argon in 100 ml of anhydrous toluene at 22° C. Octadecylmethyldichlorosilane (95%) was melted and dissolved in 100 ml of dry toluene. This solution was added dropwise at 23 to 27° C. over 55 minutes, in the course of which an exothermic reaction was observed. By cooling with an ice bath, the reaction temperature was kept at not more than 27° C. After the addition had ended, the temperature was raised to 40° C., in the course of which exothermicity (without heating to 45° C.) was again observed. The reaction vessel was then cooled to 40° C. with cold water, and the mixture was stirred at this temperature for one hour and then cooled to RT. The suspension was left to stand at RT overnight. The precipitate (hydrochloride) was filtered off with suction under N2 through a P40 glass frit, and the filtrate was concentrated by rotary evaporation at 120° C./5 mbar. Yield 80.9 g (77% of theory)

後処理

  1. temperatureIn a 1 l four-neck flask with stirrer, reflux condenser
  2. additionThis solution was added dropwise at 23 to 27° C. over 55 minutes, in the course of which
  3. customan exothermic reaction
  4. temperatureBy cooling with an ice bath
  5. customwas kept at not more than 27° C
  6. additionAfter the addition
  7. temperaturecooled to RT
  8. waitThe suspension was left
  9. waitto stand at RT overnight
  10. filtrationThe precipitate (hydrochloride) was filtered off with suction under N2 through a P40 glass frit
  11. concentrationthe filtrate was concentrated by rotary evaporation at 120° C./5 mbar

出典と根拠

ORDレコード
ord-33ff9df538b24c3b8b06d90ebf14b278
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680203B2

反応ノート

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