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

Chloroacetaldehyde → 2-(Thiazol-2-ylamino)-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-one

HRID 895986
ノート
印刷プレビュー

反応式

HRID 895986 の反応式
[O:1]=[C:2]1[NH:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[NH:5][C:4]2[CH:13]=[CH:14][C:15]([NH:17][C:18]([NH2:20])=[S:19])=[CH:16][C:3]1=2.Cl[CH2:22][CH:23]=O>C(O)C>[S:19]1[CH:23]=[CH:22][N:20]=[C:18]1[NH:17][C:15]1[CH:14]=[CH:13][C:4]2[NH:5][C:6]3[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=3[NH:8][C:2](=[O:1])[C:3]=2[CH:16]=1
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 33ChloroacetaldehydeHCID 11300593(11-Oxo-10,11-dihydro-5H-dibenzo[b,e][1,4]diazepin-2-yl)-thiourea

生成物 1

HCID 112552822-(Thiazol-2-ylamino)-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-one収率 40%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (11-oxo-10,11-dihydro-5H-dibenzo[b,e][1,4]diazepin-2-yl)-thiourea (Example 9, 75 mg, 0.26 mmol) in ethanol (10 mL) was added chloroacetaldehyde (50% in water, 0.1 mL). The solution was refluxed for 5 hr and then concentrated under vacuum and poured into water (5 mL). The solution pH was adjusted to 9 with aqueous saturated sodium bicarbonate and then extracted with ethyl acetate. The organic phase was dried over magnesium sulfate and the solvent evaporated. The residue was recrystallized from ethanol/hexanes to give yellow solid (30 mg, 40%).

後処理

  1. temperatureThe solution was refluxed for 5 hr
  2. concentrationconcentrated under vacuum
  3. additionpoured into water (5 mL)
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. customthe solvent evaporated
  7. customThe residue was recrystallized from ethanol/hexanes

出典と根拠

ORDレコード
ord-d1477a17f17a461795fa85913e690b23
出典データセット
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06919328B1

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