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Chloromethyl ethyl ether → HCID 69154097, 화합물

HRID 1296422
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HRID 1296422 반응식
[C:1]([O:4][C@H:5]([CH3:25])[CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:18](=[O:19])[C:17]2[N:16]3[CH2:20][CH2:21][NH:22][C:15]3=[N:14][C:13]=2[N:12]([CH3:23])[C:11]1=[O:24])(=[O:3])[CH3:2].C(N(C(C)C)CC)(C)C.[CH2:35]([O:37][CH2:38]Cl)[CH3:36]>C(Cl)(Cl)Cl>[C:1]([O:4][C@H:5]([CH3:25])[CH2:6][CH2:7][CH2:8][CH2:9][N:10]1[C:18](=[O:19])[C:17]2[N:16]3[CH2:20][CH2:21][N:22]([CH2:38][O:37][CH2:35][CH3:36])[C:15]3=[N:14][C:13]=2[N:12]([CH3:23])[C:11]1=[O:24])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 18523Chloromethyl ethyl etherHCID 81531DiisopropylethylamineHCID 136368748HCID 136368748, 화합물

생성물 1

HCID 69154097HCID 69154097, 화합물수율 49.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirring solution of (R)-3-(5-acetoxyhexyl)-7,8-dihydro-1-methyl-1H-imidazo[2,1-f]-purine-2,4(3H,6H)-dione (3.5 g, 10.0 mmol) and diisopropylethylamine (10.32 g, 80 mmol) in chloroform (100 ml) was added chloromethyl ethyl ether (3.78 g, 40 mmol). After stirring at room temperature for 16 hours, the reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with ethyl acetate to provide (R)-3-(5-acetoxyhexyl)-7,8-dihydro-8-ethoxymethyl-1-methyl-1H-imidazo[2,1-f]-purine-2,4(3H,6H)-dione (2.0 g, 49% yield).

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe residue was purified by column chromatography on silica gel eluting with ethyl acetate

출처 및 근거

ORD 기록
ord-16cfcf58bbbe493497ff9bd2a554b1b4
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247630B2

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