Hydrochloric Acid → 4-{[3'-(Aminomethyl)-3-(1-methyl-1H-pyrazol-5-yl)biphenyl-4-yl]oxy}-3-cyano-N-(1,3-thiazol-2-yl)benzenesulfonamide, hydrochloride salt

HRID 1619604노트

반응식

HRID 1619604 반응식
C(OC(=O)[NH:7][CH2:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]3[CH:27]=[CH:26][C:25]([S:28]([NH:31][C:32]4[S:33][CH:34]=[CH:35][N:36]=4)(=[O:30])=[O:29])=[CH:24][C:23]=3[C:37]#[N:38])=[C:17]([C:39]3[N:43]([CH3:44])[N:42]=[CH:41][CH:40]=3)[CH:16]=2)[CH:12]=[CH:13][CH:14]=1)(C)(C)C.[ClH:46]>ClCCl.O1CCOCC1>[ClH:46].[NH2:7][CH2:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]3[CH:27]=[CH:26][C:25]([S:28]([NH:31][C:32]4[S:33][CH:34]=[CH:35][N:36]=4)(=[O:29])=[O:30])=[CH:24][C:23]=3[C:37]#[N:38])=[C:17]([C:39]3[N:43]([CH3:44])[N:42]=[CH:41][CH:40]=3)[CH:16]=2)[CH:12]=[CH:13][CH:14]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 86660858HCID 86660858, 화합물

생성물 1

HCID 566013784-{[3'-(Aminomethyl)-3-(1-methyl-1H-pyrazol-5-yl)biphenyl-4-yl]oxy}-3-cyano-N-(1,3-thiazol-2-yl)benzenesulfonamide, hydrochloride salt수율 99%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

tert-Butyl-{[4′-{2-cyano-4-[(1,3-thiazol-2-ylamino)sulfonyl]phenoxy}-3′(1-methyl-1H-pyrazol-5-yl)biphenyl-3-yl]methyl}carbamate (Preparation 77, 380 mg, 0.59 mmol) was dissolved in dichloromethane (20 mL), 4M HCl in 1,4-dioxane (4 mL) was added and the reaction was stirred for 18 hours at room temperature. The reaction mixture was concentrated in vacuo, slurried in cold diethyl ether (20 ml) then filtered to afford the title compound (342 mg, 99%) as a yellow solid as the hydrochloride salt.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. filtrationthen filtered

출처 및 근거

ORD 기록
ord-64cdbdde13f84cd5a1bd6c438d8e10c9
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772293B2

반응 노트

불러오는 중…