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Triethylamine → Chlorosulfamic acid

HRID 1249688
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HRID 1249688 반응식
[Cl:1][S:2]([N:5]=C=O)(=[O:4])=[O:3].[F:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:16]([NH2:26])=[N:17][NH:18][C:19]=2[C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[CH:11][CH:10]=1.[S:27](Cl)(=[O:30])(=[O:29])[NH2:28].C(N(CC)CC)C.[OH-].[NH4+]>C1C=CC=CC=1.C(#N)C.O>[S:2]([Cl:1])(=[O:4])(=[O:3])[NH2:5].[F:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[C:16]([NH:26][S:27]([NH2:28])(=[O:30])=[O:29])=[N:17][NH:18][C:19]=2[C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 8471TriethylamineHCID 14923Ammonium HydroxideHCID 24499Chlorosulfamic acidHCID 70918Chlorosulfonyl isocyanateHCID 15428649HCID 15428649, 화합물

생성물 2

HCID 24499Chlorosulfamic acidHCID 15428653HCID 15428653, 화합물

시약·촉매·용매 3

HCID 241Benzene용매HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

Sulfamyl chloride was synthesized from chlorosulfonyl isocyanate according to the procedure described by R. Graf in Chemische Berichte, p. 509 (1959), which is incorporated herein by reference. A solution of 4-(4-fluorophenyl)-5-(4-pyridinyl)-1H-pyrazol-3-amine prepared as set forth in Example 2 (200 mg, 0.77 mmol), sulfamyl chloride (100 mg, 0.8 mmol) and triethylamine (200 mg, 2 mmol) in benzene (5 ml) and acetonitrile (5 ml) was stirred at room temperature for 2 hours. The reaction was stripped in vacuo and residue was treated with water and basified to pH 7 with ammonium hydroxide. The resultant precipitate was purified by chromatography on silica gel using mixtures of ethyl acetate and methanol as eluents. The purified [4-(4-fluorophenyl)-5-(4-pyridinyl)-1H-pyrazol-3-yl]sulfamide thus obtained had m.p. 201-202° C.

후처리

  1. customThe resultant precipitate was purified by chromatography on silica gel using mixtures of ethyl acetate and methanol as eluents

출처 및 근거

ORD 기록
ord-f130b96d69d9443eb26b3bffb1e4dd87
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06335336B1

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