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Ammonia → HCID 178453744, 화합물

HRID 1901653
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HRID 1901653 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

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

생성물 1

HCID 178453744HCID 178453744, 화합물수율 102%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3c9cfd3b50e74b4893e7ef00b3dc945c
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05578627

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