Chloroform → HCID 20337222, 화합물

HRID 2051971노트

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HRID 2051971 반응식
Br[CH2:2]/[CH:3]=[CH:4]/[P:5](=[O:16])([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].[K].[CH2:18]([O:20][C:21]([O:23][NH:24][C:25](=[O:29])[O:26][CH2:27][CH3:28])=[O:22])[CH3:19].C(Cl)(Cl)Cl>CN(C)C=O.C(OCC)(=O)C>[CH2:27]([O:26][C:25]([N:24]([CH2:2]/[CH:3]=[CH:4]/[P:5](=[O:16])([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8])[O:23][C:21]([O:20][CH2:18][CH3:19])=[O:22])=[O:29])[CH3:28]

참가 물질

7

반응물 4

HCID 6212ChloroformHCID 5462222PotassiumHCID 9995699HCID 9995699, 화합물HCID 11446651Ethyl Ethoxycarbonyloxycarbamate

생성물 1

HCID 20337222HCID 20337222, 화합물수율 39.5%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of di-tert-butyl 3-bromo-trans-1-propenylphosphonate (17.1 g.) in dry N,N-dimethylformamide (55 ml.) was added potassium salt of ethyl N-ethoxycarbonyloxycarbamate (11.03 g.). The reaction mixture was stirred for 10 minutes under ice-cooling and for 1.5 hours at ambient temperature. The reaction mixture was poured into ice water (400 ml.) and then the resultant mixture was extracted three times with ethyl acetate (300 ml., 200 ml. and 100 ml.). The combined ethyl acetate layer was washed three times with water (100 ml.), dried over magnesium sulfate and then concentrated under reduced pressure to give an oily residue (20.23 g.). The residue was subjected to column chromatography on silica gel (200 g.) [developing solvent: a mixture of chloroform and ethyl acetate (4:1)]. The fractions containing the object compound were collected and concentrated under reduced pressure to give an oily di-tert-butyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-trans- 1-propenylphosphonate (8.84 g.).

후처리

  1. extractionthe resultant mixture was extracted three times with ethyl acetate (300 ml., 200 ml. and 100 ml.)
  2. washThe combined ethyl acetate layer was washed three times with water (100 ml.)
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give an oily residue (20.23 g.)
  6. additionThe fractions containing the object compound
  7. customwere collected
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-63e0f0e9144a4b4ea1ed1580c4b8c105
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182758

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