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

Methanol → 4-[(2-Methylhydrazino)-methyl]-benzoic acid (1-hydroxymethylpropyl)-amide oxalate

HRID 1579709
ノート
印刷プレビュー

反応式

HRID 1579709 の反応式
C[N:2]([C:24](OCC1C=CC=CC=1)=O)[N:3]([CH2:14][C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1)[C:4]([O:6]CC1C=CC=CC=1)=[O:5].C(Cl)Cl.[NH2:37][CH:38]([CH2:41][CH3:42])[CH2:39][OH:40].[OH2:43].[CH3:44][OH:45]>>[C:4]([OH:6])(=[O:5])[C:44]([OH:45])=[O:43].[OH:40][CH2:39][CH:38]([NH:37][C:19](=[O:20])[C:18]1[CH:17]=[CH:16][C:15]([CH2:14][NH:3][NH:2][CH3:24])=[CH:23][CH:22]=1)[CH2:41][CH3:42]
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 5

HCID 887MethanolHCID 962WaterHCID 6344Dichloromethane2 回HCID 221292-Amino-1-butanolHCID 215690594-[(2-Methyl-1,2-dicarbobenzoxy-hydrazino)-methyl]-benzoyl chloride

生成物 1

HCID 1317098884-[(2-Methylhydrazino)-methyl]-benzoic acid (1-hydroxymethylpropyl)-amide oxalate

実験手順

15.8 g. of 4-[(2-methyl-1,2-dicarbobenzoxy-hydrazino)methyl]-benzoyl chloride were dissolved in 50 ml. of methylene chloride and, while stirring, added dropwise to a solution of 6.2 g. of 2-amino-1-butanol in 50 ml. of methylene chloride. Stirring was continued for 2 more hours at room temperature and 30 minutes at 40°, whereupon 50 ml. of water were added to the solution, which was then worked up according to Example 3. The yellowish glassy material obtained was dissolved in 200 ml. of methanol, shaken with 2 g. of 5% palladium-carbon in a hydrogen atmosphere, whereby 2/3 of the calculated amount of hydrogen had been absorbed after about 6 hours. The solution was then filtered and the filtrate concentrated in vacuo. The colorless residue was dissolved in 50 ml. of methanol and to it was added a solution of 3.2 g. of anhydrous oxalic acid in 25 ml. of methanol. Upon addition of some ether, a salt precipitated, which was recrystallized from ethanol/acetonitrile, yielding 4-[(2-methylhydrazino)-methyl]-benzoic acid (1-hydroxymethylpropyl)-amide oxalate melting at 141°-143° (dec.).

後処理

  1. additionadded dropwise to a solution of 6.2 g
  2. customThe yellowish glassy material obtained
  3. dissolutionwas dissolved in 200 ml
  4. customof 5% palladium-carbon in a hydrogen atmosphere, whereby 2/3 of the calculated amount of hydrogen had been absorbed after about 6 hours
  5. filtrationThe solution was then filtered
  6. concentrationthe filtrate concentrated in vacuo
  7. dissolutionThe colorless residue was dissolved in 50 ml
  8. additionof methanol and to it was added a solution of 3.2 g
  9. additionUpon addition of some ether
  10. customa salt precipitated
  11. customwhich was recrystallized from ethanol/acetonitrile

出典と根拠

ORDレコード
ord-32cf10e61be44698ab29bb87b73c1bf5
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931268

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