Ethyl bromoacetate → HCID 13338732, 화합물

HRID 485670노트

반응식

HRID 485670 반응식
[N:1]([CH:4]1[CH2:12][CH2:11][CH2:10][CH2:9][C:8]2[CH:13]=[CH:14][CH:15]=[CH:16][C:7]=2[NH:6][C:5]1=[O:17])=[N+:2]=[N-:3].CC(C)([O-])C.[K+].Br[CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27]>CN(C)C=O>[N:1]([CH:4]1[CH2:12][CH2:11][CH2:10][CH2:9][C:8]2[CH:13]=[CH:14][CH:15]=[CH:16][C:7]=2[N:6]([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])[C:5]1=[O:17])=[N+:2]=[N-:3]

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 13338731HCID 13338731, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 13338732HCID 13338732, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

A solution of 3-azido-1,3,4,5,6,7-hexahydro-1-benzazonin-2-one (8.9 g) in dry dimethylformamide (100 ml) is added during 30 minutes to a solution of potassium t-butoxide (4.5 g) in dry dimethylformamide (100 ml) maintained at 0° under an atmosphere of dry nitrogen. The reaction mixture is stirred at 0° for 2 hours, when a solution of ethyl bromoacetate (5.8 g) in dimethylformamide (10 ml) is added during 5 minutes. The reaction mixture is stirred at 0° for 2 hours, then evaporated under reduced pressure. The residue is distributed between ethyl acetate (250 ml) and water (150 ml), and the ethyl acetate solution washed with water (100 ml) and dried over sodium sulfate. The solvent is removed under reduced pressure to give 3-azido-1-ethoxycarbonylmethyl-1,3,4,5,6,7-hexahydro-1-benzazonin-2-one.

후처리

  1. temperaturemaintained at 0° under an atmosphere of dry nitrogen
  2. stirringThe reaction mixture is stirred at 0° for 2 hours
  3. customevaporated under reduced pressure
  4. washthe ethyl acetate solution washed with water (100 ml)
  5. dry with materialdried over sodium sulfate
  6. customThe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-da8be1d2d8214dbd9b0ed27eb1c3bc49
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04537885

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