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Sodium hydride → HCID 86637534, 화합물

HRID 1099107
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HRID 1099107 반응식
[OH:1][C@@H:2]1[CH2:6][CH2:5][O:4][CH2:3]1.[H-].[Na+].Cl[C:10]1[C:11]2[N:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:12]=2[N:13]=[C:14]([NH:16]C(=O)C)[N:15]=1>C1COCC1>[Cl:24][C:22]1[CH:21]=[CH:20][C:12]2[N:13]=[C:14]([NH2:16])[N:15]=[C:10]([O:1][CH:2]3[CH2:6][CH2:5][O:4][CH2:3]3)[C:11]=2[N:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 641512(-)-3-HydroxytetrahydrofuranHCID 57698319N-(4,6-Dichloropyrido[3,2-d]pyrimidin-2-yl)acetamide

생성물 1

HCID 86637534HCID 86637534, 화합물수율 51%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

(R)-(−)-3-hydroxy-tetrahydrofuran (0.62 mL) was added to a suspension of NaH (0.31 g, 7.7 mmol) in THF (15 mL). After stirring for 1 hour, the resulting mixture was added to a suspension of N-(4,6-dichloro-pyrido[3,2-d]pyrimidin-2-yl)-acetamide (0.9 g, 3.5 mmol) in THF (15 mL). The mixture was stirred at room temperature for 20 minutes, then diluted with EtOAC (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated to afford 6-chloro-4-(tetrahydro-furan-3-yloxy)-pyrido[3,2-d]pyrimidin-2-ylamine as a yellow solid (0.55 g, yield: 51%) which was characterized by its mass spectrum as follows: MS (m/z) 309.1 [M+H]+.

후처리

  1. stirringThe mixture was stirred at room temperature for 20 minutes
  2. additiondiluted with EtOAC (100 mL)
  3. washwashed with brine
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9c8f69c9c93c4ea29e2512d97429a096
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08143394B2

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