Triethylamine → HCID 13885366、化合物

HRID 2232020ノート

反応式

HRID 2232020 の反応式
[F:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11](Cl)(=[O:13])=[O:12])(=[O:4])=[O:3].[NH:15]1[CH2:18][CH2:17][CH2:16]1.C(N(CC)CC)C>C(#N)C>[N:15]1([S:11]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[S:2]([F:1])(=[O:4])=[O:3])(=[O:13])=[O:12])[CH2:18][CH2:17][CH2:16]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10422AzetidineHCID 976312-Fluorosulphonylbenzenesulphonyl chloride

生成物 1

HCID 13885366HCID 13885366、化合物収率 100.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

In a flask was placed 9.24 g of 2-fluorosulfonylbenzenesulfonyl chloride and 200 ml of dry acetonitrile. The resultant solution was cooled to 0° C. An addition funnel was charged with 2 g of azetidine, 4.95 ml of triethylamine and 50 ml of acetonitrile. This solution was added dropwise to the first solution. After stirring overnight the solvent was evaporated under reduced pressure. The residue was partitioned between dichloromethane and 1N hydrochloric acid. The organic layer was separated, dried and concentrated to give 9.80 g of a solid, m.p. 93° C.

後処理

  1. customIn a flask was placed
  2. additionThis solution was added dropwise to the first solution
  3. customwas evaporated under reduced pressure
  4. customThe residue was partitioned between dichloromethane and 1N hydrochloric acid
  5. customThe organic layer was separated
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-9b8977cf11df402ba2ef64eab96b2caf
出典データセット
uspto-grants-1988_11
特許番号
US04786316

反応ノート

読み込み中…