Dimethylformamide dimethyl acetal → N,N-Dimethyl-N'-(5-bromothiophene-2-sulfonyl)formamidine

HRID 2414128노트

반응식

HRID 2414128 반응식
[Br:1][C:2]1[S:6][C:5]([S:7]([NH2:10])(=[O:9])=[O:8])=[CH:4][CH:3]=1.CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>C(#N)C>[CH3:13][N:14]([CH3:16])[CH:15]=[N:10][S:7]([C:5]1[S:6][C:2]([Br:1])=[CH:3][CH:4]=1)(=[O:9])=[O:8]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 12413045-Bromo-2-thiophenesulfonamide

생성물 1

HCID 54319951N,N-Dimethyl-N'-(5-bromothiophene-2-sulfonyl)formamidine

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To a stirred mixture of 5-bromothiophene-2-sulfonamide (24.2 g, 0.10 mol) in acetonitrile (100 ml) was added dimethylformamide dimethyl acetal (14 ml) in acetonitrile (125 ml) dropwise over 0.5 hour. After an additional 0.5 hour the solvent was removed in vacuo. The residue was treated with water and the solid that precipitated was collected and dried, 28.7 g., m.p. 103°-105° C. Recrystallization from 1-chlorobutane gave material with m.p. 104°-106° C.

후처리

  1. customAfter an additional 0.5 hour the solvent was removed in vacuo
  2. additionThe residue was treated with water
  3. customthe solid that precipitated
  4. customwas collected
  5. customdried
  6. customRecrystallization from 1-chlorobutane
  7. customgave material with m.p. 104°-106° C.

출처 및 근거

ORD 기록
ord-b5ae77c898774c65b6c661607a2c8528
출처 데이터셋
uspto-grants-1988_01
특허 번호
US04721794

반응 노트

불러오는 중…