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Sodium Iodide → 1-(3-(5-Chloro-2,3-dihydrospiro[indene-1,3'-pyrrolidine]-1'-yl)propyl)-5-(thiophen-2-yl)pyrimidine-2,4(1h,3h)-dione hydrochloride

HRID 1661081
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HRID 1661081 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[CH:10]=[C:9]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)[C:8](=[O:16])[NH:7][C:6]1=[O:17].Cl.[Cl:19][C:20]1[CH:21]=[C:22]2[C:30](=[CH:31][CH:32]=1)[C:25]1([CH2:29][CH2:28][NH:27][CH2:26]1)[CH2:24][CH2:23]2.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>O.CN1C(=O)CCC1>[ClH:1].[Cl:19][C:20]1[CH:21]=[C:22]2[C:30](=[CH:31][CH:32]=1)[C:25]1([CH2:29][CH2:28][N:27]([CH2:2][CH2:3][CH2:4][N:5]3[CH:10]=[C:9]([C:11]4[S:12][CH:13]=[CH:14][CH:15]=4)[C:8](=[O:16])[NH:7][C:6]3=[O:17])[CH2:26]1)[CH2:24][CH2:23]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 593375931-(3-chloropropyl)-5-(2-thienyl)-2,4(1H,3H)-pyrimidinedioneHCID 674279925-Chloro-2,3-dihydrospiro[indene-1,3'-pyrrolidine] hydrochloride

생성물 1

HCID 674297191-(3-(5-Chloro-2,3-dihydrospiro[indene-1,3'-pyrrolidine]-1'-yl)propyl)-5-(thiophen-2-yl)pyrimidine-2,4(1h,3h)-dione hydrochloride수율 81.3%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

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온도
70 °C

실험 절차

A mixture of 1-(3-chloropropyl)-5-(thiophen-2-yl)pyrimidine-2,4(1H,3H)-dione (Prep24, 50 mg, 0.18 mmol), 5-chloro-2,3-dihydrospiro[indene-1,3′-pyrrolidine]hydrochloride salt (Prep10, 66 mg, 0.27 mmol), potassium carbonate (112 mg, 0.81 mmol), sodium iodide (112 mg, 0.75 mmol) and NMP (1 ml) was stirred at 70° C. overnight. Then it was cooled down to room temperature and diluted with water and extracted with ethyl acetate. The EA phase was evaporated and the crude purified by preparative TLC (TLC analysis performed by eluting with EA/MeOH 10:1) to give the free base of the title compound (70 mg). The compound was purified by preparative HPLC and treated with a 1N solution of HCl-ether to give the title compound (9 mg, y=10%).

후처리

  1. temperatureThen it was cooled down to room temperature
  2. extractionextracted with ethyl acetate
  3. customThe EA phase was evaporated
  4. customthe crude purified by preparative TLC (TLC analysis performed by eluting with EA/MeOH 10:1)

출처 및 근거

ORD 기록
ord-3b11f6e5cd354543a48dc77cdd1079c6
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030322B2

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