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Tert-Butylamine → (E)-tert-butyl-(3,4-dihydro-2H-pyran-2-yl-methylene)-amine

HRID 1248522
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인쇄 미리보기

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HRID 1248522 반응식
[CH2:1]1[CH:6]=[CH:5][O:4][CH:3]([CH:7]=O)[CH2:2]1.[C:9]([NH2:13])([CH3:12])([CH3:11])[CH3:10]>C(O)C>[CH3:10][C:9]([N:13]=[CH:7][CH:3]1[CH2:2][CH2:1][CH:6]=[CH:5][O:4]1)([CH3:12])[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6385Tert-ButylamineHCID 60994Acrolein dimer

생성물 1

HCID 13476808(E)-tert-butyl-(3,4-dihydro-2H-pyran-2-yl-methylene)-amine

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 323.0 g of acrolein dimer in 230 ml of anhydrous ethanol was added dropwise to a solution of 251 ml of t-butylamine in 250 ml of anhydrous ethanol at 25° C. over 2 hours. The reaction mixture was stirred at room temperature overnight. The solvents were stripped off on a rotary evaporator to leave 295.5 g of a yellow oil. This oil was vacuum distilled at 8 mm Hg to give 223 g of a colorless oil at 63°-67° C. and four fractions of colorless oil were collected as follows: 2.82 g at 45°-63° C., 181.27 g at 63°-66° C., 42.42 g at 66°-67° C. and 37.09 g at 67°-70° C., and were a mixture of isomers of the desired product.

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후처리

  1. customThe solvents were stripped off on a rotary evaporator

출처 및 근거

ORD 기록
ord-3492c7a11cae47ac848ca624b7e1df67
출처 데이터셋
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04525203

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