Triethylamine → HCID 13885366, 화합물

HRID 1906347노트

반응식

HRID 1906347 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10422AzetidineHCID 976312-Fluorosulphonylbenzenesulphonyl chloride

생성물 1

HCID 13885366HCID 13885366, 화합물수율 100.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e87d32659a4243828f00f0d3e96cd17e
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04652304

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