3-Mercaptopropionic Acid → Cgp 20376

HRID 1980821노트

반응식

HRID 1980821 반응식
[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]

참가 물질

4

반응물 2

HCID 65143-Mercaptopropionic AcidHCID 173314Cgp 20308

생성물 1

HCID 3035447Cgp 20376

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-58d5566a531f40cf94847592fe4896db
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04511567

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