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Boron tribromide → HCID 19918009, 화합물

HRID 1755871
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HRID 1755871 반응식
C([O:8][C:9]1[C:10](=[O:29])[N:11]([CH3:28])[C:12]([CH2:15][O:16][N:17]2[C:21](=[O:22])[C:20]3=[CH:23][CH:24]=[CH:25][CH:26]=[C:19]3[C:18]2=[O:27])=[N:13][CH:14]=1)C1C=CC=CC=1.B(Br)(Br)Br>ClCCl>[OH:8][C:9]1[C:10](=[O:29])[N:11]([CH3:28])[C:12]([CH2:15][O:16][N:17]2[C:21](=[O:22])[C:20]3=[CH:23][CH:24]=[CH:25][CH:26]=[C:19]3[C:18]2=[O:27])=[N:13][CH:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 19917833N-[[5-(benzyloxy)-3,4-dihydro-3-methyl-4-oxo-2-pyrimidinyl]methoxy]phthalimide

생성물 1

HCID 19918009HCID 19918009, 화합물수율 91.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-70 °C

실험 절차

N-[[5-(Benzyloxy)-3,4-dihydro-3-methyl-4-oxo-2-pyrimidinyl]methoxy]phthalimide (1.56 g) (4 mmol) are dissolved in 110 ml of dichloromethane and treated dropwise at about -70° C. while stirring with 0.42 ml (4.4 mmol) of boron tribromide. After stirring at about -70° C. for 4 hours and at room temperature for 16 hours the solvent is removed in a water-jet vacuum at room temperature. The residue is treated with about 30 ml of water, the insoluble product is filtered off and washed firstly with water and subsequently with diethyl ether. After drying in a high vacuum at room temperature for 18 hours there are obtained 1.1 g of N-[(3,4-dihydro-5-hydroxy-3-methyl-4-oxo-2-pyrimidinyl)methoxy]phthalimide as a white powder, m.p. 172° C. (dec.).

후처리

  1. additiontreated dropwise at about -70° C.
  2. customis removed in a water-jet vacuum at room temperature
  3. additionThe residue is treated with about 30 ml of water
  4. filtrationthe insoluble product is filtered off
  5. washwashed firstly with water and subsequently with diethyl ether
  6. customAfter drying in a high vacuum at room temperature for 18 hours there

출처 및 근거

ORD 기록
ord-2ecbe721c55b497ba8e6792ce42527bb
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05438052

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