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Triethylamine → HCID 178490722、化合物

HRID 641275
ノート
印刷プレビュー

反応式

HRID 641275 の反応式
[ClH:1].[NH2:2][OH:3].C(N(CC)CC)C.[C:11]([C:13]1[CH:18]=[CH:17][C:16]([NH:19][C:20]([C:22]2[CH:23]=[CH:24][C:25]3[O:30][CH2:29][CH2:28][N:27]([S:31]([C:34]4[CH:39]=[C:38](Cl)[CH:37]=[CH:36][C:35]=4[O:41][CH3:42])(=[O:33])=[O:32])[C:26]=3[CH:43]=2)=[O:21])=[CH:15][CH:14]=1)#[N:12]>CS(C)=O.O>[OH:3][NH:2][C:11]([C:13]1[CH:14]=[CH:15][C:16]([NH:19][C:20]([C:22]2[CH:23]=[CH:24][C:25]3[O:30][CH2:29][CH2:28][N:27]([S:31]([C:34]4[CH:39]=[C:38]([Cl:1])[CH:37]=[CH:36][C:35]=4[O:41][CH3:42])(=[O:32])=[O:33])[C:26]=3[CH:43]=2)=[O:21])=[CH:17][CH:18]=1)=[NH:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 667886204-(5-chloro-2-methoxy-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazine-6-carboxylic acid (4-cyano-phenyl)-amide

生成物 1

HCID 178490722HCID 178490722、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒

実験手順

A solution of hydroxylamine hydrochloride (90 mg, 1.3 mmol) in dimethyl sulfoxide (1.25 mL) was treated with triethylamine (131 mg, 0.18 mL, 1.3 mmol) and stirred at room temperature for 5 min. The solids were filtered off, and 4-(5-chloro-2-methoxy-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazine-6-carboxylic acid (4-cyano-phenyl)-amide (125 mg, 0.26 mmol) was added. The mixture was stirred at 75° C. for 1.5 hours. After cooling back to room temperature, the mixture was diluted with water and extracted with ethyl acetate. The organic phase was extracted three times with 0.5N HCl. The combined acidic aqueous layer was then rebasified with 1N NaOH and extracted three times with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate and evaporated. 4-(5-Chloro-2-methoxy-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazine-6-carboxylic acid [4-(N-hydroxycarbamimidoyl)-phenyl]-amide was obtained as a white solid, 97 mg (73%), MS (ISP): m/e=517.0 (M+H+.).

後処理

  1. filtrationThe solids were filtered off
  2. stirringThe mixture was stirred at 75° C. for 1.5 hours
  3. temperatureAfter cooling back to room temperature
  4. extractionextracted with ethyl acetate
  5. extractionThe organic phase was extracted three times with 0.5N HCl
  6. extractionextracted three times with ethyl acetate
  7. washThe organic layer was washed with water
  8. dry with materialdried over sodium sulfate
  9. customevaporated

出典と根拠

ORDレコード
ord-d33176ccaa714c3a9febb1bdb607c2c4
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07696200B2

反応ノート

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