Sodium Sulfate → 1-Dodecylazepane

HRID 981454

반응식

HRID 981454 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°/0.03 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°/0.03 mm)

출처 및 근거

ORD 기록
ord-a4ab3fbc760d4c649a4daf7fb67026be
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04992422

연결된 노트

불러오는 중…