Sodium Methoxide → 4-Propyl-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide

HRID 743450노트

반응식

HRID 743450 반응식
C[O:2][C:3](=O)[C:4]([CH2:11][CH2:12][CH3:13])(C)[NH:5][S:6]([NH2:9])(=[O:8])=[O:7].[CH3:15][O-].[Na+]>CO>[CH2:11]([CH:4]1[N:5]([CH3:15])[S:6](=[O:8])(=[O:7])[NH:9][C:3]1=[O:2])[CH2:12][CH3:13]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 19424444N-aminosulfonyl-2-propyl-DL-alanine methyl ester

생성물 1

HCID 189222534-Propyl-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide수율 125.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of N-(aminosulfonyl)-2-propyl-DL-alanine methyl ester (10.66 g; 47.53 mmol) in methanol (100 ml) was added in one portion to a solution of sodium methoxide (prepared from 2.0 g of Na in 100 ml of dry methanol under nitrogen) and the resulting reaction mixture was stirred for 15 hours. The mixture was neutralized with BIO-RAD® 50W-X8 H+ ion exchange resin with stirring (20 minutes), and filtered. The filtrate was concentrated in vacuo to yield an oil which was dried in vacuo (4 hours) to afford 8.96 g (98%) of 4-methyl-4-propyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide (Formula IV: R1 =propyl;R2 =CH3 ; R3 =H).

후처리

  1. customthe resulting reaction mixture
  2. stirringwith stirring (20 minutes)
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto yield an oil which
  6. customwas dried in vacuo (4 hours)

출처 및 근거

ORD 기록
ord-e4b8a906673643eabff1ab02aa953ca0
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556909

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