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Piperidine → HCID 86747749, 화합물

HRID 128566
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HRID 128566 반응식
[S:1](/[CH:4]=[CH:5]\[C:6]([OH:8])=O)[C:2]#[N:3].C(N(CC)CC)C.ClC(OCC)=O.[NH:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1>C1(C)C=CC=CC=1>[S:1](/[CH:4]=[CH:5]\[C:6]([N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1)=[O:8])[C:2]#[N:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8082PiperidineHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 53838152-Propenoic acid, 3-thiocyanato-

생성물 1

HCID 86747749HCID 86747749, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매4회

실험 절차

To a stirred suspension of compound 2 (3.06 g., 0.023 mole) in 60 ml of dry toluene, triethylamine (2.35 g., 0.023 mole) in 10 ml of dry toluene was added dropwise, keeping the temperature of the mixture at 0°-5° C. To the resulting solution was added dropwise, ethyl chloroformate (2.53 g., 0.023 mole) in 15 ml of dry toluene at 0°-5° C. After stirring the mixture for 15 minutes, piperidine (2.0 g., 0.023 mole) in 15 ml of dry toluene was added dropwise at 0°-5° C. The mixture was allowed to warm to room temperature, stirred for an additional 2 hours and filtered. The filtrate was washed with water, dried (MgSO4) and concentrated to give an oil which solidified, 2.6 g. The solid was recrystallized from ethanol: mp 88°-90° C.; IR (KBr) 2175, 1630 cm-1

후처리

  1. additionwas added dropwise
  2. customat 0°-5° C
  3. additionTo the resulting solution was added dropwise
  4. customat 0°-5° C
  5. stirringstirred for an additional 2 hours
  6. filtrationfiltered
  7. washThe filtrate was washed with water
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated
  10. customto give an oil which
  11. customThe solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-ffd5ec8a63004ca0af41101db072720c
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05464832

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