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Iodine chloride → HCID 86723847, 화합물

HRID 576746
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HRID 576746 반응식
[OH:1][CH2:2][C@H:3]([N:5]1[C:10](=[O:11])[CH:9]=[CH:8][N:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[C:6]1=[O:22])[CH3:4].[I:23]Cl>C(Cl)(Cl)Cl>[OH:1][CH2:2][C@H:3]([N:5]1[C:10](=[O:11])[C:9]([I:23])=[CH:8][N:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:19])[F:20])[CH:13]=2)[C:6]1=[O:22])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24640Iodine chlorideHCID 86723846HCID 86723846, 화합물

생성물 1

HCID 86723847HCID 86723847, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of (R)-3-(1-hydroxypropan-2-yl)-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (prepared in Reference Example 102) (1.3 g) in chloroform (20.0 ml) was added iodine chloride (12.4 ml, 1M dichloromethane solution) and the resulting mixture was stirred for two hours at room temperature. The reaction mixture was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate) to afford (R)-3-(1-hydroxypropan-2-yl)-5-iodo-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (1.4 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-a4fef27cf4da4e639d009bf9d9802953
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040516B2

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