Sodium Carbonate → 3-[[2-(4-Thiomorpholinyl)ethyl]amino]-1,2-benzisoxazol-6-ol

HRID 582878노트

반응식

HRID 582878 반응식
COC[O:4][C:5]1[CH:22]=[CH:21][C:8]2[C:9]([NH:12][CH2:13][CH2:14][N:15]3[CH2:20][CH2:19][S:18][CH2:17][CH2:16]3)=[N:10][O:11][C:7]=2[CH:6]=1.C([O-])([O-])=O.[Na+].[Na+]>Cl>[N:15]1([CH2:14][CH2:13][NH:12][C:9]2[C:8]3[CH:21]=[CH:22][C:5]([OH:4])=[CH:6][C:7]=3[O:11][N:10]=2)[CH2:20][CH2:19][S:18][CH2:17][CH2:16]1

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 154351386-Methoxymethoxy-N-[2-(4-thiomorpholinyl)ethyl]-1,2-benzisoxazol-3-amine

생성물 1

HCID 1358150603-[[2-(4-Thiomorpholinyl)ethyl]amino]-1,2-benzisoxazol-6-ol수율 72.4%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

6-Methoxymethoxy-N-[2-(4-thiomorpholinyl)ethyl]-1,2-benzisoxazol-3-amine (1.6 g Example 22) was dissolved in methanolic hydrochloric acid (40 ml) and stirred under nitrogen for 24 hours. The reaction was neutralized with saturated Na2CO3 solution, and extracted with EtOAc. The organic phase was dried over MgSO4 and concentrated in vacuo. The resulting residue was filtered through a silica gel filter-cake eluting with 5% MeOH/DCM, concentrated in vacuo, and subsequent titration with EtOAc provided the product (1.0 g).

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe organic phase was dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. filtrationThe resulting residue was filtered through a silica gel
  5. filtrationfilter-cake
  6. washeluting with 5% MeOH/DCM
  7. concentrationconcentrated in vacuo, and subsequent titration with EtOAc

출처 및 근거

ORD 기록
ord-f422f283ead54167a6953f64d395c33c
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925766

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