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Hydrogen chloride-ethyl acetate → 1-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2, 4-dione dihydrochloride

HRID 1183089
ノート
印刷プレビュー

反応式

HRID 1183089 の反応式
C(OC(=O)C)C.[ClH:7].[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([O:26][CH2:27][CH2:28][CH2:29][NH:30][CH2:31][CH2:32][C:33]3[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=3)[CH:24]=[CH:25][C:11]1=2)[CH3:9]>C(OCC)(=O)C>[ClH:7].[ClH:7].[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([O:26][CH2:27][CH2:28][CH2:29][NH:30][CH2:31][CH2:32][C:33]3[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=3)[CH:24]=[CH:25][C:11]1=2)[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 686730021-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino) propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

生成物 1

HCID 686735041-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2, 4-dione dihydrochloride収率 85%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A 4N-hydrogen chloride ethyl acetate solution (0.37 ml) was added to an ethyl acetate solution (10 ml) of 1-ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (207 mg, 0.49 mmol), and stirred for 30 minutes at room temperature. The precipitated insoluble matter was collected by filtration, washed with ethyl acetate, and dried to thereby obtain 208 mg (yield: 85%) of 1-ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione dihydrochloride as a pale yellow amorphous solid.

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-abe31ad30f9b40e6a1a6346784fa6c60
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664217B2

反応ノート

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