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

Diisopropylethylamine → 1-Amino-3-(4-carboxyphenyl)-2-thioxoimidazolidin-4-one

HRID 555626
ノート
印刷プレビュー

反応式

HRID 555626 の反応式
[N:1]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)=[C:2]=[S:3].C(N(C(C)C)CC)(C)C.Cl.[NH:23]([CH2:25][C:26](OCC)=[O:27])[NH2:24]>ClCCl>[NH2:24][N:23]1[CH2:25][C:26](=[O:27])[N:1]([C:4]2[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=2)[C:2]1=[S:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 2429464-Isothiocyanatobenzoic acidHCID 11593468Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1)

生成物 1

HCID 859639971-Amino-3-(4-carboxyphenyl)-2-thioxoimidazolidin-4-one収率 53%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

179 mg (1 mmol) of 4-isothiocyanatobenzoic acid and 523 μl (3 mmol) of diisopropylethylamine were stirred in 8 ml of dichloromethane and then with 155 mg (1 mmol) of ethyl hydrazinoacetate hydrochloride at room temperature for 96 hours. After the solvent was concentrated, the mixture was partitioned between ethyl acetate and 30% acetic acid. The aqueous layer was extracted with ethyl acetate again, and the organic layers were combined, washed with water and then with saturated aqueous sodium chloride, dried over magnesium sulfate and concentrated. The resulting solid was mixed with a 190:10:0.8 liquid mixture of ethyl acetate, methanol and acetic acid, and the insoluble was dried to obtain 132 mg of the desired product (yield 53%).

後処理

  1. concentrationAfter the solvent was concentrated
  2. customthe mixture was partitioned between ethyl acetate and 30% acetic acid
  3. extractionThe aqueous layer was extracted with ethyl acetate again
  4. washwashed with water
  5. dry with materialwith saturated aqueous sodium chloride, dried over magnesium sulfate
  6. concentrationconcentrated
  7. additionThe resulting solid was mixed with a 190:10:0.8 liquid mixture of ethyl acetate, methanol and acetic acid
  8. customthe insoluble was dried

出典と根拠

ORDレコード
ord-c629cad49e724fefb1e59aa5b27806bb
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08053453B2

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