3-Mercaptopropionic Acid → Cgp 20376

HRID 1980821ノート

反応式

HRID 1980821 の反応式
[C:1]([C:5]1[S:6][C:7]2[CH:13]=[C:12]([N:14]=[C:15]=[S:16])[C:11]([O:17][CH3:18])=[CH:10][C:8]=2[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[SH:19][CH2:20][CH2:21][C:22]([OH:24])=[O:23]>CN(C)C=O>[C:22]([CH2:21][CH2:20][S:19][C:15](=[S:16])[NH:14][C:12]1[C:11]([O:17][CH3:18])=[CH:10][C:8]2[N:9]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[S:6][C:7]=2[CH:13]=1)([OH:24])=[O:23]

参加物

4

反応物 2

HCID 65143-Mercaptopropionic AcidHCID 173314Cgp 20308

生成物 1

HCID 3035447Cgp 20376

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

27.8 g (0.10 mole) of 2-tert.-butyl-6-isothiocyano-5-methoxy-benzthiazole are dissolved in 150 ml of dimethylformamide and 14 g (0.13 mole) of 3-mercaptopropionic acid are added. The solution is stirred at room temperature under nitrogen for 2 hours, then poured onto 2 kg of ice and stirred until the product has become solid. It is filtered off, washed with water and heated in 700 ml of toluene, decanted from water, dried over sodium sulphate, clarified with active carbon and filtered. The filtrate is diluted at 30-40° with approximately 700 ml of petroleum ether and cooled slowly to 5°, filtered off and subsequently washed with petroleum ether. N-[2-tert.-butyl-5-methoxy-benzthiazol-6-yl]-dithiocarbamic acid S-(2-carboxyethyl)-ester having a melting point of 154-156° is obtained: ##STR14##

後処理

  1. stirringstirred until the product
  2. filtrationIt is filtered off
  3. washwashed with water
  4. temperatureheated in 700 ml of toluene
  5. customdecanted from water
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. additionThe filtrate is diluted at 30-40° with approximately 700 ml of petroleum ether
  9. temperaturecooled slowly to 5°
  10. filtrationfiltered off
  11. washsubsequently washed with petroleum ether

出典と根拠

ORDレコード
ord-58d5566a531f40cf94847592fe4896db
出典データセット
uspto-grants-1985_04
特許番号
US04511567

反応ノート

読み込み中…