Bromine → 3-Bromo-1-dodecylazacycloheptan-2-one

HRID 845101

반응식

HRID 845101 반응식
[CH2:1]([N:13]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]1=[O:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].P(Cl)(Cl)(Cl)(Cl)Cl.[Br:27]Br>C(Cl)(Cl)Cl>[Br:27][CH:15]1[CH2:16][CH2:17][CH2:18][CH2:19][N:13]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:14]1=[O:20]

참가 물질

5

반응물 3

HCID 24408BromineHCID 24819Phosphorus pentachlorideHCID 42981Laurocapram

생성물 1

HCID 141826953-Bromo-1-dodecylazacycloheptan-2-one

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a cold solution of 107 g (0.38 mol) of 1-dodecylazacycloheptan-2-one, in CHCl3 was added 159.7 g (0.77 mol) of PCl5, keeping the temperature between 1°-4° C. After 2 hours, a solution of 123.3 g (0.77 mol) of bromine in CHCl3 was added, and the mixture was stirred for 18 hours at room temperature. After removing the solvent and excess bromine by vacuum distillation, the residue was dissolved in CH2Cl2, washed with sat. Na2S2O5, dried over MgSO4, and concentrated in vacuo to give a crude oil. Purification by flash chromatography (silica gel; 1:1 ether/petroleum ether V/V) gave pure product.

후처리

  1. custombetween 1°-4° C
  2. customAfter removing the solvent and excess bromine
  3. distillationby vacuum distillation
  4. dissolutionthe residue was dissolved in CH2Cl2
  5. washwashed with sat. Na2S2O5
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customto give a crude oil
  9. customPurification by flash chromatography (silica gel; 1:1 ether/petroleum ether V/V)
  10. customgave pure product

출처 및 근거

ORD 기록
ord-24c5b0f902134d598ede491cde24c195
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04755535

연결된 노트

불러오는 중…