ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Triethylamine → HCID 178490722、化合物

HRID 1360243
ノート
印刷プレビュー

反応式

HRID 1360243 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-e3841050fd814a91bfe293359b8eb38d
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879845B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート