홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → HCID 131731068, 화합물

HRID 1192453
노트
인쇄 미리보기

반응식

HRID 1192453 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 5146Salicyl AlcoholHCID 78835Silane, dichloromethyloctadecyl-HCID 81531Diisopropylethylamine

생성물 1

HCID 131731068HCID 131731068, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
45 °C

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-33ff9df538b24c3b8b06d90ebf14b278
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680203B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트