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

2,6-Diphenylpiperidine → 1,4-Bis(2,6-diphenylpiperidin-1-yl)-2-butene

HRID 1590798
노트
인쇄 미리보기

반응식

HRID 1590798 반응식
[C:1]1([CH:7]2[CH2:12][CH2:11][CH2:10][CH:9]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>O1CCCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:13]1([CH:9]2[CH2:10][CH2:11][CH2:12][CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]2[CH2:6][CH:1]=[CH:2][CH2:3][N:8]2[CH:9]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:10][CH2:11][CH2:12][CH:7]2[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 130106382,6-Diphenylpiperidine

생성물 1

HCID 543523251,4-Bis(2,6-diphenylpiperidin-1-yl)-2-butene수율 61%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2,6-diphenylpiperidine [3.0 g, 12.6 mmol; prepared by the method of V. Baliah et al., Indian J. Chem., 16B, 1965 (1978)] and 1,4-but-2-enediol diacetate (1.1 g, 6.3 mmol) in tetrahydrofuran (20 ml, THF) is treated with tetrakis(triphenylphosphine)palladium (0) (0.65 g, 0.6 mmol) and stirred at room temperature overnight. The reaction mixture is concentrated in vacuo to a solid that is redissolved in THF (100 ml) and treated with 20% aqueous sodium hydroxide (25 ml). The mixture is stirred for one hour, concentrated, and extracted with diethyl ether. The ether extracts are dried and concentrated giving an orange solid which is purified by crystallization from methanol to yield 2.02 g (61%) of the title compound as a white solid melting at 197°-200° C.

후처리

  1. customprepared by the method of V
  2. concentrationThe reaction mixture is concentrated in vacuo to a solid
  3. dissolutionthat is redissolved in THF (100 ml)
  4. additiontreated with 20% aqueous sodium hydroxide (25 ml)
  5. stirringThe mixture is stirred for one hour
  6. concentrationconcentrated
  7. extractionextracted with diethyl ether
  8. dry with materialThe ether extracts are dried
  9. concentrationconcentrated
  10. customgiving an orange solid which
  11. customis purified by crystallization from methanol

출처 및 근거

ORD 기록
ord-57f9b17eac8e4ab8b6b9ee4b6028c6c3
출처 데이터셋
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05204474

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트