2,3,4,5-Tetrahydro-1,5-benzoxazepine → 5-Nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine

HRID 50981

반응식

HRID 50981 반응식
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[NH:5][CH2:4][CH2:3][CH2:2]1.[N:12]([O-])=[O:13].[Na+]>Cl.O>[N:12]([N:5]1[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[O:1][CH2:2][CH2:3][CH2:4]1)=[O:13]

참가 물질

5

반응물 2

HCID 5777522,3,4,5-Tetrahydro-1,5-benzoxazepineHCID 23668193Sodium Nitrite

생성물 1

HCID 122337995-Nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine수율 95.1%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매2회

실험 절차

To a stirred, cold slurry of 2,3,4,5-tetrahydro-1,5-benzoxazepine (13.72 g, 91.96 mmol) in 2N aqueous HCl (105 mL) was added dropwise a solution of NaNO2 (7.30 g, 105.75 mmol) in H2O (16 mL) and stirred at room temperature for 2 hrs. The mixture was taken up in H2O (800 mL), extracted with ether (3×200 mL), dried over MgSO4, and stripped of the solvent under reduced pressure to yield 15.59 g (95%) of 5-nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine as a tan powder. (M+H)+ 178.

후처리

  1. extractionextracted with ether (3×200 mL)
  2. dry with materialdried over MgSO4

출처 및 근거

ORD 기록
ord-54e9657d3fcb4bd3becb32aee40351a7
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713471B1

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