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4-Methylmorpholine → 9-Dodecen-1-ol

HRID 542637
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HRID 542637 반응식
[CH2:1]([OH:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][C:9]#[C:10][CH2:11][CH3:12].CN1CCOCC1.C([O-])([O-])=O.[Ca+2]>CO.[Pd].[Zn]>[CH2:1]([OH:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]=[CH:10][CH2:11][CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 79724-MethylmorpholineHCID 10112Calcium CarbonateHCID 1170119-Dodecyn-1-ol

생성물 1

HCID 931819-Dodecen-1-ol수율 96.7%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 23994Zinc촉매HCID 887
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
Methanol
용매

실험 절차

6212 g (34.8 moles) of dodec-9-yn-1-ol and 316 g of N-methylmorpholine are dissolved in 46 l of methanol in a 100 l glass flask, and 62 g of a catalyst (0.7% Pd and 3.1% of Zn on a CaCO3 carrier) are suspended in the solution. Thereafter, the stirred suspension is flushed with nitrogen, and hydrogenation is carried out at from 0° to 5° C. and under a hydrogen pressure of 0.1 bar above atmospheric pressure until the absorption of hydrogen is complete. The methanol and morpholine are stripped off to give 6,200 g of dodec-9-en-1-ol containing 96.6% of the cis compound and 2.1% of the trans compound.

후처리

  1. customThereafter, the stirred suspension is flushed with nitrogen, and hydrogenation
  2. customis carried out at from 0° to 5° C. and under a hydrogen
  3. customuntil the absorption of hydrogen

출처 및 근거

ORD 기록
ord-7e104de1ac1c4e399322e34f397b2efb
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04658071

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