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Hydrochloric Acid → heptadecane, 3-methyl-

HRID 2380171
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HRID 2380171 반응식
[CH3:1][CH:2]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[C:3](=O)[CH3:4].O.NN.[OH-].[Na+].Cl>O.C(O)COCCO>[CH3:1][CH:2]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[CH2:3][CH3:4]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 15376167HCID 15376167, 화합물

생성물 1

HCID 94321heptadecane, 3-methyl-수율 53%

시약·촉매·용매 2

HCID 962Water용매
HCID 8117
Diethylene Glycol
용매

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온도
200 °C

실험 절차

2 g (7.46 mmol) of 3-methyl-heptadecan-2-one (Compound No. 3 of Table 1) are introduced into 10 ml of diethylene glycol, and the mixture is treated with 1.11 g (22.4 mmol) of hydrazine hydrate and 1.2 g (29.85 mmol) of sodium hydroxide. The mixture is stirred for twenty hours at 200° C. When the mixture has cooled to room temperature, it is treated with 100 ml of water, acidified with hydrochloric acid, with cooling, and extracted three times using cyclohexane. The combined organic extracts are washed twice with a little water, dried over sodium sulphate and concentrated. Separation by column chromatography using cyclohexane as the eluent gave 1.0 g (53% of theory) of 3-methylheptadecane.

후처리

  1. temperatureWhen the mixture has cooled to room temperature
  2. temperaturewith cooling
  3. extractionextracted three times
  4. washThe combined organic extracts are washed twice with a little water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. customSeparation by column chromatography

출처 및 근거

ORD 기록
ord-8acf9980d905422eab83c4207ba7eae7
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05365691

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