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Phosphorus oxychloride → HCID 20080518, 화합물

HRID 1653824
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HRID 1653824 반응식
P(Cl)(Cl)(Cl)=O.[C:6]1([C:12](=[O:32])[CH:13]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[NH:14][C:15](=O)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH:21]([C:23]#[N:24])[CH3:22])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C1(C)C=CC=CC=1>[C:26]1([C:13]2[N:14]=[C:15]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH:21]([CH3:22])[C:23]#[N:24])[O:32][C:12]=2[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 20080542HCID 20080542, 화합물

생성물 1

HCID 20080518HCID 20080518, 화합물수율 76.9%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

7.3 g of phosphorus oxychloride are added to a solution of 5.75 g of (RS)-1,2-diphenyl-2-(7-cyanooctanamido)ethanone in 30 cm3 of toluene, and the mixture is heated to 80° C. for 6 hours. After treatment, the product obtained is chromatographed on a column 2 cm in diameter containing 60 g of silica gel (50 to 200μ). The column is eluted with 0.6 liter of diisopropyl ether, collecting 50 cm3 fractions. The fractions emerging at between 0.1 liter and 0.6 liter are concentrated under reduced pressure (0.2 kPa). 4.2 g (76%) of (RS)-7-(4,5-diphenyl-2-oxazolyl)-2-methylheptanenitrile are obtained in the form of an oil, which is used directly in the subsequent reaction.

후처리

  1. customAfter treatment, the product obtained
  2. customis chromatographed on a column 2 cm in diameter
  3. additioncontaining 60 g of silica gel (50 to 200μ)
  4. washThe column is eluted with 0.6 liter of diisopropyl ether
  5. customcollecting 50 cm3 fractions
  6. concentrationare concentrated under reduced pressure (0.2 kPa)

출처 및 근거

ORD 기록
ord-7d6541a0dcc043b99c0e9ac1e1a5013b
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05403852

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