Ethyl bromoacetate → HCID 13338732、化合物

HRID 485670ノート

反応式

HRID 485670 の反応式
[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]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 13338731HCID 13338731、化合物HCID 23665647Potassium tert-butoxide

生成物 1

HCID 13338732HCID 13338732、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-da8be1d2d8214dbd9b0ed27eb1c3bc49
出典データセット
uspto-grants-1985_08
特許番号
US04537885

反応ノート

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