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

HRID 1080436ノート

反応式

HRID 1080436 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-08dfa34cf8e64502a75ad770fd4c80c7
出典データセット
uspto-grants-1996_12
特許番号
US05580982

反応ノート

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