Hydrogen Cyanide → 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin

HRID 267767

반응식

HRID 267767 반응식
[O:1]=[C:2]1[CH2:8][O:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[O:4][CH2:3]1.[CH:13]#[N:14].C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC=CC=1>[OH:1][C:2]1([C:13]#[N:14])[CH2:3][O:4][C:5]2[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=2[O:7][CH2:8]1

참가 물질

5

반응물 3

HCID 768Hydrogen CyanideHCID 10340Sodium CarbonateHCID 113097002H-1,5-Benzodioxepin-3(4H)-one

생성물 1

HCID 155572933-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a stirred solution of 4.92 g. (30 millimoles) of 3-oxo-3,4-dihydro-2H-1,5-benzodioxepin in 100 mls. of benzene is added dropwise a solution of 30 millimoles of anhydrous hydrogen cyanide in 50 ml. of benzene. The reaction mixture is stirred overnight at ambient temperature, basified with 10% sodium carbonate solution and the organic layer separated. The benzene solution is washed once with water and dried successively over anhydrous magnesium sulfate and calcium sulfate. Evaporation of the solvent under reduced pressure at 40° C. yields the crude cyanohydrin which upon purification and mixed melting point determination gives no depression with an authentic sample of 3-hydroxy-3-cyano-3,4-dihydro-2H-1,5-benzodioxepin.

후처리

  1. customthe organic layer separated
  2. washThe benzene solution is washed once with water
  3. dry with materialdried successively over anhydrous magnesium sulfate and calcium sulfate
  4. customEvaporation of the solvent under reduced pressure at 40° C.
  5. customyields the crude cyanohydrin which
  6. customupon purification
  7. additionmixed

출처 및 근거

ORD 기록
ord-e6799d215004407bbdec444fa4284f11
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03944560

연결된 노트

불러오는 중…