Benzenesulfonic Acid → HCID 140636156, 화합물

HRID 715743노트

반응식

HRID 715743 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 140636156HCID 140636156, 화합물

시약·촉매·용매 1

HCID 7915Isopropyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f566975d5f864797ba6769ed37962efc
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187488B2

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