Sodium Sulfate → 1-Dodecylazepane

HRID 1587477

반응식

HRID 1587477 반응식
[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[CH2:1]([N:13]1[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 42981LaurocapramHCID 21226445Aluminium lithium hydride

생성물 1

HCID 33661291-Dodecylazepane수율 93.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

56.2g (0.2 mol) of 1-dodecylazacycloheptan-2-one in 100ml diethyl ether was added dropwise to a suspension of 7.6g (0.2 mol) lithium aluminum hydride in 100ml diethyl ether under argon at room temperature. After 5 hours of stirring, 20ml saturated sodium sulfate was added dropwise. The mixture was filtered and the filtrate was dried with magnesium sulfate, filtered and concentrated. The resulting oil was distilled (130°/.03 mm) to yield 50.03g (93.5%) of 1-n-dodecylazacycloheptane.

후처리

  1. filtrationThe mixture was filtered
  2. dry with materialthe filtrate was dried with magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. distillationThe resulting oil was distilled (130°/.03 mm)

출처 및 근거

ORD 기록
ord-124f3113283747acbf5f492760bd94d0
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05218113

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