Hydrochloric Acid → HCID 15908472, 화합물

HRID 480026노트

반응식

HRID 480026 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 95884-Fluorobenzenesulfonyl chlorideHCID 18768328HCID 18768328, 화합물

생성물 1

HCID 15908472HCID 15908472, 화합물수율 34.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-2d358a7a2aff40029844bc40a68edc6b
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649618B2

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