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 1619604ノート

反応式

HRID 1619604 の反応式
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

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 86660858HCID 86660858、化合物

生成物 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 salt収率 99%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-64cdbdde13f84cd5a1bd6c438d8e10c9
出典データセット
uspto-grants-2014_07
特許番号
US08772293B2

反応ノート

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