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Hydrochloric Acid → N-[4-(5,6,7,8-Tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl)phenyl]methanesulfonamide

HRID 1364131
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HRID 1364131 반응식
[CH3:1][S:2]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:21]=[C:20]3[C:14]([CH2:15][CH2:16][N:17](C(OC(C)(C)C)=O)[CH2:18][CH2:19]3)=[N:13]2)=[CH:8][CH:7]=1)(=[O:4])=[O:3].Cl>O1CCOCC1.CO>[N:13]1[N:12]([C:9]2[CH:8]=[CH:7][C:6]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:11][CH:10]=2)[CH:21]=[C:20]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15][C:14]=12
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 669308081,1-Dimethylethyl 2-{4-[(methylsulfonyl)amino]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate

생성물 1

HCID 66930788N-[4-(5,6,7,8-Tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl)phenyl]methanesulfonamide

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of 1,1-dimethylethyl 2-{4-[(methylsulfonyl)amino]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate (may be prepared as described in Description 39) (16 mg, 0.039 mmol) in dioxan (1 ml) was added 4M hydrochloric acid in dioxan (2 ml). The resulting mixture was stirred at room temperature, under argon, overnight. The reaction mixture was diluted with methanol and then purified by SCX, eluting with methanol and then 2M ammonia/methanol. The basic fractions were combined and solvent evaporated in vacuo to afford the title compound (D40). MS (ES+) m/e 307 [M+H]+.

후처리

  1. custompurified by SCX
  2. washeluting with methanol
  3. customsolvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-c42726a43a1b4ea6989e606bfb2eb298
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07888347B2

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