4-(Aminosulfonyl)-3-thiophenecarbonyl chloride → 4-(Aminosulfonyl)-N-[3-[3-(1-piperidinylcarbonyl)phenoxy]propyl]-3-thiophene-carboxamide, hydrate

HRID 1731413노트

반응식

HRID 1731413 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([C:12]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=[O:13])[CH:9]=[CH:10][CH:11]=1.[NH2:20][S:21]([C:24]1[C:25]([C:29](Cl)=[O:30])=[CH:26][S:27][CH:28]=1)(=[O:23])=[O:22]>O1CCCC1>[OH2:5].[NH2:20][S:21]([C:24]1[C:25]([C:29]([NH:1][CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:11]=[CH:10][CH:9]=[C:8]([C:12]([N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)=[O:13])[CH:7]=2)=[O:30])=[CH:26][S:27][CH:28]=1)(=[O:23])=[O:22]

참가 물질

4

반응물 2

HCID 137325564-(Aminosulfonyl)-3-thiophenecarbonyl chlorideHCID 137325581-[[3-(3-Aminopropoxy)phenyl]carbonyl]piperidine

생성물 1

HCID 1317149444-(Aminosulfonyl)-N-[3-[3-(1-piperidinylcarbonyl)phenoxy]propyl]-3-thiophene-carboxamide, hydrate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 0.26 g. (0.001 mole) of 1-[[3-(3-aminopropoxy)phenyl]carbonyl]piperidine in 30 ml. of dry tetrahydrofuran is added 0.23 g. (0.001 mole) of 4-(aminosulfonyl)-3-thiophenecarbonyl chloride. The mixture is allowed to stand at room temperature for 15 minutes. The tetrahydrofuran is removed in a rotary evaporator and the residue is dissolved in 50 ml. of chloroform. The chloroform solution is extracted with 50 ml. of 10% aqueous sodium hydroxide solution followed by 50 ml. of 10% aqueous hydrochloric acid. The chloroform layer is washed with water, is dried over magnesium sulfate and is filtered. The filtrate is evaporated in a rotary evaporator to give 0.15 g. of an amorphous product, m.p. 70°-80° C.; mass spectrum CI m/e 452 MH+.

후처리

  1. customThe tetrahydrofuran is removed in a rotary evaporator
  2. dissolutionthe residue is dissolved in 50 ml
  3. extractionThe chloroform solution is extracted with 50 ml
  4. washThe chloroform layer is washed with water
  5. dry with materialis dried over magnesium sulfate
  6. filtrationis filtered
  7. customThe filtrate is evaporated in a rotary evaporator
  8. customto give 0.15 g

출처 및 근거

ORD 기록
ord-b9392de950984e5d9ebc3d61483ea14f
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04621142

반응 노트

불러오는 중…