Diphosgene → HCID 23368411、化合物

HRID 1901606ノート

反応式

HRID 1901606 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][OH:23])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl[C:25](OC(Cl)(Cl)Cl)=[O:26].Cl.[CH3:33][O:34][NH2:35].C[O-].[Na+]>C(Cl)Cl.CO.O.C(N(CC)CC)C>[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][O:23][C:25]([NH:35][O:34][CH3:33])=[O:26])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

9

反応物 4

HCID 10426DiphosgeneHCID 521874O-Methylhydroxylamine hydrochlorideHCID 10942334Sodium MethoxideHCID 233683553-(2-Tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole

生成物 1

HCID 23368411HCID 23368411、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

実験手順

A solution of 1.00 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-chloro-1,2-benzoisoxazole and 0.73 g of triethylamine in 5 ml of methylene chloride is added to a solution of 0.42 g of trichloromethyl chloroformate in 5 ml of methylene chloride at 5°-7° C. over 20 minutes, and they are subjected to reaction at the same temperature for 30 minutes. This solution is added to a solution of 1.20 g of methoxyamine hydrochloride and 0.78 g of sodium methoxide in 15 ml of methanol at -30° C. and the temperature is elevated to 0° C., at which they are subjected to reaction for 30 minutes. Water is added to the reaction mixture, and after shaking, the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure to obtain 3-(2-tert-butoxycarbonylamino-3-methoxyaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole.

後処理

  1. customthey are subjected to reaction at the same temperature for 30 minutes
  2. customis elevated to 0° C., at which they
  3. customare subjected to reaction for 30 minutes
  4. customthe organic layer is separated
  5. washThe separated organic layer is washed with a saturated saline solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customafter which the solvent is removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-df896198371b4813ba46ae7695f190de
出典データセット
uspto-grants-1996_11
特許番号
US05578627

反応ノート

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