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Hydrazine hydrate (1:1) → 3,6,9,12,15-Pentaoxaheptadecane-1,17-diamine

HRID 1279175
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HRID 1279175 반응식
C1(=O)[N:5]([CH2:6][CH2:7][O:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][O:14][CH2:15][CH2:16][O:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][N:23]2C(=O)C3=CC=CC=C3C2=O)C(=O)C2=CC=CC=C12.O.NN>C(O)C>[NH2:23][CH2:22][CH2:21][O:20][CH2:19][CH2:18][O:17][CH2:16][CH2:15][O:14][CH2:13][CH2:12][O:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][NH2:5]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 18427234HCID 18427234, 화합물

생성물 1

HCID 156101913,6,9,12,15-Pentaoxaheptadecane-1,17-diamine수율 97.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °C

실험 절차

The synthesis generally followed the method of Kern et al., Makrol. Chem., 180, 2539 (1979). A solution containing 60 g of 1,17-diphthalimido-3,6,9,12,15-pentaoxaheptadecane (0.118 mol), 14.8 g of hydrazine hydrate (0.296 mol), and 500 mL of ethanol is heated with mechanical stirring in a 100° C. oil bath for three hrs. The mixture is cooled and filtered. A resultant filter cake is washed four times with 300 mL portions of ethanol. The combined filtrates are concentrated to yield 32.35 g of a yellow opaque glassy oil by evaporative distillation at 150-200° C. (0.01 mm of vacuum). The result is 22.82 g of a light yellow oil (69% yield). b.p. 175-177° C. (0.07 mm).

후처리

  1. customThe synthesis
  2. temperatureis heated
  3. temperatureThe mixture is cooled
  4. filtrationfiltered
  5. filtrationA resultant filter cake
  6. washis washed four times with 300 mL portions of ethanol
  7. concentrationThe combined filtrates are concentrated

출처 및 근거

ORD 기록
ord-5a7066d196a2471487373230fff0da29
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06448047B2

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