Hydrochloric Acid → HCID 15908472、化合物

HRID 480026ノート

反応式

HRID 480026 の反応式
[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][N:6]1[C:15]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=2[C:9](=[O:16])[NH:8][C:7]1=[O:17].[F:18][C:19]1[CH:24]=[CH:23][C:22]([S:25](Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1.Cl>N1C=CC=CC=1>[O:17]=[C:7]1[NH:8][C:9](=[O:16])[C:10]2[CH2:11][CH2:12][CH2:13][CH2:14][C:15]=2[N:6]1[CH2:5][CH2:4][CH2:3][N:2]([CH3:1])[S:25]([C:22]1[CH:23]=[CH:24][C:19]([F:18])=[CH:20][CH:21]=1)(=[O:27])=[O:26]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 95884-Fluorobenzenesulfonyl chlorideHCID 18768328HCID 18768328、化合物

生成物 1

HCID 15908472HCID 15908472、化合物収率 34.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 75 mg (0.32 mmol) of 1-[3-(methylamino)propyl]-5,6,7,8-tetrahydro-2,4(1H,3H)-quinazolinedione and 61.5 mg (0.32 mmol) of 4-fluorophenylsulphonyl chloride in 3 ml of pyridine is stirred at room temperature overnight. The reaction mixture is then adjusted to pH 1 using 2-molar hydrochloric acid and extracted twice with in each case 20 ml of ethyl acetate. The organic phase is concentrated under reduced pressure and the resulting residue is purified by preparative HPLC (RP-C18, acetonitrile/water gradient). This gives 43.1 mg (34% yield) of the product as an amorphous solid.

後処理

  1. extractionextracted twice with in each case 20 ml of ethyl acetate
  2. concentrationThe organic phase is concentrated under reduced pressure
  3. customthe resulting residue is purified by preparative HPLC (RP-C18, acetonitrile/water gradient)

出典と根拠

ORDレコード
ord-2d358a7a2aff40029844bc40a68edc6b
出典データセット
uspto-grants-2003_11
特許番号
US06649618B2

反応ノート

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