Sodium Methoxide → 4-(3-Methylbutyl)-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide

HRID 1450461노트

반응식

HRID 1450461 반응식
C[O:2][C:3](=O)[CH:4]([CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[N:5]([S:7]([NH2:10])(=[O:9])=[O:8])[CH3:6].C[O-].[Na+]>CO>[CH3:14][CH:13]([CH3:15])[CH2:12][CH2:11][CH:4]1[N:5]([CH3:6])[S:7](=[O:9])(=[O:8])[NH:10][C:3]1=[O:2]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 18922252N-(aminosulfonyl)-2-(3-methylbutyl)sarcosine methyl ester

생성물 1

HCID 189222624-(3-Methylbutyl)-5-methyl-1,2,5-thiadiazolidin-3-one 1,1-dioxide수율 100.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of N-(aminosulfonyl)-2-(3-methylbutyl)sarcosine methyl ester (12.25 g, 48.17 mmol) in methanol (150 ml) was added to a solution of sodium methoxide (Na=2.4 g) in 150 ml of ice-cold methanol. The resulting reaction mixture was stirred at room temperature under nitrogen for 18.5 hours, and then the mixture was treated with 25 g of ion-exchange resin (BIO RAD® 50W x 8; 200-400 mesh) for 40 minutes and filtered. The filtrate was concentrated in vacuo to afford 10.7 g (99.8%) of 4- (3-methylbutyl)-5-methyl--1,2,5-thiadiazolidin-3-one 1,1-dioxide (Formula IV: R1 =(CH2)2CH(CH3)2 ; R2 =H; R3 =CH3) as a solid, m.p. 212°-214° C.

후처리

  1. customThe resulting reaction mixture
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-8b1a0d8971c1470781343ced040724e7
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602154

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