Tetrahydrofuran → 3,3-Diethoxy-1-propanol

HRID 1848676노트

반응식

HRID 1848676 반응식
O1CCCC1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:12]([O:14][CH:15]([O:22][CH2:23][CH3:24])[CH2:16][C:17](OCC)=[O:18])[CH3:13]>O>[CH2:12]([O:14][CH:15]([O:22][CH2:23][CH3:24])[CH2:16][CH2:17][OH:18])[CH3:13]

참가 물질

5

반응물 3

HCID 8028Tetrahydrofuran2회HCID 66389Ethyl 3,3-diethoxypropionateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 1401353,3-Diethoxy-1-propanol수율 109.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

In the following, tetrahydrofuran (THF) to be used was dehydrated on molecular sieves of 4 angstrom overnight. Inside of a 5 L four-neck flask was substituted with nitrogen gas and 2.2 kg of THF was placed therein, followed by cooling to 10° C. or lower. Then, 50 g of lithium aluminum hydride was placed therein and 250 g of ethyl 3,3-diethoxypropionate was added dropwise so that inner temperature did not exceed 10° C. After completion of the dropwise addition, temperature was elevated to 20° C. and reaction was carried out for 1 hour. After the reaction, 420 g of distilled water was added and the whole was stirred for 2 hours, then filtration was performed through No. 2 filtration paper, and subsequently a cake was washed with 1.1 kg of THF. The filtrate was concentrated at 40° C. to obtain 213 g of crude 3,3-diethoxy-1-propanol (hereinafter 33DEP).

후처리

  1. customto be used was dehydrated on molecular sieves of 4 angstrom overnight
  2. customdid not exceed 10° C
  3. additionAfter completion of the dropwise addition, temperature
  4. customwas elevated to 20° C.
  5. customreaction
  6. additionwas added
  7. filtrationfiltration
  8. filtration2 filtration paper
  9. washsubsequently a cake was washed with 1.1 kg of THF
  10. concentrationThe filtrate was concentrated at 40° C.

출처 및 근거

ORD 기록
ord-e17e15b67a784746bec1d38aee0679ab
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952203B2

반응 노트

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