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Hydrochloric Acid → N,N-dimethyl-1-[6-(1-naphthylsulfonyl)-2,3-dihydro[1,4]oxazino[2,3,4-hi]indazol-2-yl]methanamine Hydrochloride

HRID 33111
ノート
印刷プレビュー

反応式

HRID 33111 の反応式
[Cl:1][CH2:2][CH:3]1[CH2:13][N:12]2[C:14]3[C:9]([C:10]([S:15]([C:18]4[C:27]5[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=5)[CH:21]=[CH:20][CH:19]=4)(=[O:17])=[O:16])=[N:11]2)=[CH:8][CH:7]=[CH:6][C:5]=3[O:4]1.[CH3:28][NH:29][CH3:30].Cl.CCOCC>CS(C)=O.O>[ClH:1].[CH3:28][N:29]([CH3:30])[CH2:2][CH:3]1[O:4][C:5]2=[C:14]3[C:9](=[CH:8][CH:7]=[CH:6]2)[C:10]([S:15]([C:18]2[C:27]4[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=4)[CH:21]=[CH:20][CH:19]=2)(=[O:17])=[O:16])=[N:11][N:12]3[CH2:13]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 3283Diethyl EtherHCID 251690347-Chloromethyl-2(naphthalene-1-sulfonyl)-7,8-dihydro-6-oxa-1,8a-diaza-acenaphthylene

生成物 1

HCID 25169296N,N-dimethyl-1-[6-(1-naphthylsulfonyl)-2,3-dihydro[1,4]oxazino[2,3,4-hi]indazol-2-yl]methanamine Hydrochloride

試薬・触媒・溶媒 2

HCID 679
Dimethyl Sulfoxide
溶媒
HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of 7-chloromethyl-2-(naphthalene-1-sulfonyl)-7,8-dihydro-6-oxa-1,8a-diaza-acenaphthylene (0.075 g, 0.18 mmoles) and dimethylamine (0.56 ml, 1M solution in THF, 0.56 mmoles) in DMSO was stirred under nitrogen at 100° C. for 4 hours, cooled to room temperature, diluted with water and extracted with EtOAc. The extracts were combined, washed sequentially with water and brine, dried over Na2SO4 and concentrated under vacuum. The resultant residue was purified by flash chromatography using as eluent 5% CH3OH/EtOAc. The purified compound was dissolved in methanol, treated with 1M HCl in ether (0.2 ml, 0.2 mmoles) and evaporated to dryness to afford the title compound, MS: (ES) m/z 407.

後処理

  1. temperaturecooled to room temperature
  2. extractionextracted with EtOAc
  3. washwashed sequentially with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under vacuum
  6. customThe resultant residue was purified by flash chromatography
  7. dissolutionThe purified compound was dissolved in methanol
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-54107132d07d48338dc750a18208c17c
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429582B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート