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

HRID 2414128ノート

反応式

HRID 2414128 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-b5ae77c898774c65b6c661607a2c8528
出典データセット
uspto-grants-1988_01
特許番号
US04721794

反応ノート

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