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

HRID 1731413ノート

反応式

HRID 1731413 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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+.

後処理

  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

出典と根拠

ORDレコード
ord-b9392de950984e5d9ebc3d61483ea14f
出典データセット
uspto-grants-1986_11
特許番号
US04621142

反応ノート

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