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Ammonia → HCID 178453744、化合物

HRID 1901653
ノート
印刷プレビュー

反応式

HRID 1901653 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][C:23]1[O:27][N:26]=[C:25]([O:28]S(C2C=CC=CC=2)(=O)=O)[CH:24]=1)[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].CO.N.Cl>O1CCCC1.C(OCC)(=O)C.O>[C:1]([O:5][C:6]([NH:8][CH:9]([CH2:22][C:23]1[O:27][N:26]=[C:25]([OH:28])[CH:24]=1)[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])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 887MethanolHCID 233684903-[2-Tert-butoxycarbonylamino-3-(3-benzenesulfonyloxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole

生成物 1

HCID 178453744HCID 178453744、化合物収率 102%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 0.5 g of 3-[2-tert-butoxycarbonylamino-3-(3-benzenesulfonyloxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole in 4 ml of tetrahydrofuran is added 2.5 ml of a methanol solution (6N) of ammonia at room temperature, and they are subjected to reaction at the same temperature for 16 hours. Water and ethyl acetate are added to the reaction mixture, 1N hydrochloric acid is thereafter added to adjust the pH to 2, 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 0.38 g of 3-[2-tert-butoxycarbonylamino-3-(3-hydroxy-5-isoxazolyl)propoxy]-5-chloro-1,2-benzoisoxazole having a melting point of 158.8°-160.7° C.

後処理

  1. customthey are subjected to reaction at the same temperature for 16 hours
  2. additionis thereafter added
  3. customthe organic layer is separated
  4. washThe separated organic layer is washed with a saturated saline solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter which the solvent is removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-3c9cfd3b50e74b4893e7ef00b3dc945c
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05578627

反応ノート

読み込み中…

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