Hydrogen chloride-ethyl acetate → 2-Nitro-n-(2-pyridin-3-ylethyl)-n-[3-(1,3,3,5-tetramethyl-2,4-dioxo-2,3,4,5-tetrahydro-1h-benzo[b][1,4]diazepin-7-yloxy)propyl]benzenesulfonamide hydrochloride

HRID 2196076ノート

反応式

HRID 2196076 の反応式
C(OC(=O)C)C.[ClH:7].[N+:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S:17]([N:20]([CH2:42][CH2:43][C:44]1[CH:45]=[N:46][CH:47]=[CH:48][CH:49]=1)[CH2:21][CH2:22][CH2:23][O:24][C:25]1[CH:41]=[CH:40][C:28]2[N:29]([CH3:39])[C:30](=[O:38])[C:31]([CH3:37])([CH3:36])[C:32](=[O:35])[N:33]([CH3:34])[C:27]=2[CH:26]=1)(=[O:19])=[O:18])([O-:10])=[O:9]>C(OCC)(=O)C>[ClH:7].[N+:8]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[S:17]([N:20]([CH2:42][CH2:43][C:44]1[CH:45]=[N:46][CH:47]=[CH:48][CH:49]=1)[CH2:21][CH2:22][CH2:23][O:24][C:25]1[CH:41]=[CH:40][C:28]2[N:29]([CH3:39])[C:30](=[O:38])[C:31]([CH3:36])([CH3:37])[C:32](=[O:35])[N:33]([CH3:34])[C:27]=2[CH:26]=1)(=[O:18])=[O:19])([O-:10])=[O:9]

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 686742442-nitro-N-(2-pyridin-3-ylethyl)-N-[3-(1,3,3,5-tetramethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yloxy)propyl]benzenesulfonamide

生成物 1

HCID 686743582-Nitro-n-(2-pyridin-3-ylethyl)-n-[3-(1,3,3,5-tetramethyl-2,4-dioxo-2,3,4,5-tetrahydro-1h-benzo[b][1,4]diazepin-7-yloxy)propyl]benzenesulfonamide hydrochloride収率 65%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A 4N-hydrogen chloride ethyl acetate solution (0.57 ml) was added to an ethyl acetate solution (1 ml) of 2-nitro-N-(2-pyridin-3-ylethyl)-N-[3-(1,3,3,5-tetramethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yloxy)propyl]benzenesulfonamide (236 mg), and stirred at room temperature for 1 minute. The precipitated insoluble matter was collected by filtration, washed with ethyl acetate, and dried to thereby obtain 163 mg (yield: 65%) of 2-nitro-N-(2-pyridin-3-ylethyl)-N-[3-(1,3,3,5-tetramethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yloxy)propyl]benzenesulfonamide hydrochloride as a white powder.

後処理

  1. filtrationThe precipitated insoluble matter was collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

出典と根拠

ORDレコード
ord-72d656e3077b43a99710c5a9c40ef885
出典データセット
uspto-grants-2012_12
特許番号
US08338406B2

反応ノート

読み込み中…