Benzenesulfonic Acid → HCID 140636156、化合物

HRID 715743ノート

反応式

HRID 715743 の反応式
[CH3:1][S:2]([N:5]1[CH:9]=[C:8]2[CH2:10][N:11](C(OC(C)(C)C)=O)[CH2:12][C:7]2=[N:6]1)(=[O:4])=[O:3].[C:20]1([S:26]([OH:29])(=[O:28])=[O:27])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(OC(=O)C)(C)C>[C:20]1([S:26]([O-:29])(=[O:28])=[O:27])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[CH3:1][S:2]([N:5]1[CH:9]=[C:8]2[CH2:10][NH2+:11][CH2:12][C:7]2=[N:6]1)(=[O:3])=[O:4]

参加物

4

反応物 2

HCID 7371Benzenesulfonic AcidHCID 711512761,1-Dimethylethyl 2,6-dihydro-2-(methylsulfonyl)pyrrolo[3,4-c]pyrazole-5(4H)-carboxylate

生成物 1

HCID 140636156HCID 140636156、化合物

試薬・触媒・溶媒 1

HCID 7915Isopropyl Acetate溶媒

実験手順

To a solution of tert-butyl 2-(methylsulfonyl)-2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-carboxylate (32.1 kg, 111 mol) in iso-propylacetate (289 kg) was added benzenesulfonic acid (35.35 kg, 223 mol). The reaction was stirred for 3 days at room temperature and then cooled to 0-10° C. and stirred an additional 1 h. The resulting slurry was filtered and the cake washed with iso-propylacetate. The solids were dried overnight under vacuum at room temperature to give 2-(methylsulfonyl)-2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-5-ium benzenesulfonate.

後処理

  1. temperaturecooled to 0-10° C.
  2. stirringstirred an additional 1 h
  3. filtrationThe resulting slurry was filtered
  4. washthe cake washed with iso-propylacetate
  5. customThe solids were dried overnight under vacuum at room temperature

出典と根拠

ORDレコード
ord-f566975d5f864797ba6769ed37962efc
出典データセット
uspto-grants-2015_11
特許番号
US09187488B2

反応ノート

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