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4,6-Dichloro-n-methylpyrimidin-2-amine → 4-Chloro-6-[(2R)-2-ethyl-1-pyrrolidinyl]-N-methyl-2-pyrimidinamine

HRID 2367631
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인쇄 미리보기

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HRID 2367631 반응식
[CH2:1]([C@@H:3]1[CH2:7][CH2:6][CH2:5][NH:4]1)[CH3:2].[Cl:8][C:9]1[CH:14]=[C:13](Cl)[N:12]=[C:11]([NH:16][CH3:17])[N:10]=1>O1CCOCC1.C([O-])(O)=O.[Na+]>[Cl:8][C:9]1[CH:14]=[C:13]([N:4]2[CH2:5][CH2:6][CH2:7][C@H:3]2[CH2:1][CH3:2])[N:12]=[C:11]([NH:16][CH3:17])[N:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2598804,6-Dichloro-n-methylpyrimidin-2-amineHCID 10931375(R)-2-ethylpyrrolidine

생성물 1

HCID 585045454-Chloro-6-[(2R)-2-ethyl-1-pyrrolidinyl]-N-methyl-2-pyrimidinamine수율 88.3%

시약·촉매·용매 2

HCID 312751,4-Dioxane용매HCID 516892Sodium Bicarbonate용매

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온도
100 °C

실험 절차

A mixture of (2R)-2-ethylpyrrolidine (0.8 g, 5.90 mmol) and 4,6-dichloro-N-methyl-2-pyrimidinamine (0.997 g, 5.60 mmol) in 1,4-dioxane (40 mL) and saturated aqueous NaHCO3 (20 mL) was stirred overnight at 100° C. into a sealed tube. The reaction mixture was poured onto water (˜400 mL). A white precipitate was formed. The aqueous mixture was filtered, and the white solid was washed with water (˜100 mL). The wet solid was dried overnight on vacuum at 40° C. to afford the title compound (1.19 g). LC-MS (ES) m/z=241 [M+H]+.

후처리

  1. additionThe reaction mixture was poured onto water (˜400 mL)
  2. customA white precipitate was formed
  3. filtrationThe aqueous mixture was filtered
  4. washthe white solid was washed with water (˜100 mL)
  5. customThe wet solid was dried overnight on vacuum at 40° C.

출처 및 근거

ORD 기록
ord-0ce5a86eeaa9494f8732a6a98ddb3471
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697685B2

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