Diisopropyl Ether → HCID 20337244, 화합물

HRID 2051968노트

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HRID 2051968 반응식
[CH2:1]([O:8][N:9]([CH2:20][CH2:21]Br)[S:10]([C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=1)(=[O:12])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[P:23]([O:30]CC)([O:27][CH2:28][CH3:29])[O:24][CH2:25][CH3:26].C(OCC)(=O)C.C(OC(C)C)(C)C>O>[CH2:1]([O:8][N:9]([CH2:20][CH2:21][P:23](=[O:30])([O:27][CH2:28][CH3:29])[O:24][CH2:25][CH3:26])[S:10]([C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=1)(=[O:12])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 7914Diisopropyl EtherHCID 8857Ethyl AcetateHCID 31215Triethyl phosphiteHCID 20337232HCID 20337232, 화합물

생성물 1

HCID 20337244HCID 20337244, 화합물수율 57%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
160 °C

실험 절차

A mixture of N-benzyloxy-N-(2-bromoethyl)-p-toluenesulfonamide (16.2 g.) and triethyl phosphite (21.0 g.) was stirred at 160° C. for 10 hours and then cooled to ambient temperature. To the reaction mixture was added ethyl acetate and water. The ethyl acetate layer was separated, washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give an oily residue (20.5 g.). A small volume of isopropyl ether was added to the residue to give crystals, which was separated by filtration and dried to give crystalline diethyl 2-(N-benzyloxy-N-tosylamino)ethylphosphonate (10.6 g.). The object compound (2.1 g.) was also recovered from the mother liquor by subjecting to a column chromatography on silicagel (developing solvent: chloroform)

후처리

  1. temperaturecooled to ambient temperature
  2. customThe ethyl acetate layer was separated
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give an oily residue (20.5 g.)
  7. customto give crystals, which
  8. customwas separated by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-0719c68507954fe48823f15363f2de45
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182758

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