Sodium hydride → HCID 22639999, 화합물

HRID 2415098

반응식

HRID 2415098 반응식
[NH2:1][C:2]1[C:7]([Cl:8])=[C:6]([CH3:9])[N:5]=[C:4]([CH3:10])[N:3]=1.[CH2:11]([O:18][C:19]1[CH:20]=[C:21]([CH:24]=[CH:25][C:26]=1[O:27][CH3:28])[CH2:22]Cl)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[H-].[Na+]>CN1CCCC1=O>[CH2:11]([O:18][C:19]1[CH:20]=[C:21]([CH:24]=[CH:25][C:26]=1[O:27][CH3:28])[CH2:22][NH:1][C:2]1[C:7]([Cl:8])=[C:6]([CH3:9])[N:5]=[C:4]([CH3:10])[N:3]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2802242-(Benzyloxy)-4-(chloromethyl)-1-methoxybenzeneHCID 5938434-Amino-5-chloro-2,6-dimethylpyrimidine

생성물 1

HCID 22639999HCID 22639999, 화합물

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

In analogy to the method described in example A1, 6.11 g (38 mmol) of 4-amino-5-chloro-2,6-dimethylpyrimidine, 10.5 g (40 mmol) of 3-benzyloxy-4-methoxybenzyl chloride and 1.52 g (38 mmol) of sodium hydride (60% suspension in liquid paraffin) are reacted in a total of 225 ml of N-methylpyrrolidone. After chromatography on silica gel (mobile phase: toluene/dioxane=10:1) and crystallization from petroleum ether, the title compound is isolated as a pale beige solid. Yield: 5.2 g (36% of theory). m.p.: 111-117° C.

후처리

  1. customAfter chromatography on silica gel (mobile phase: toluene/dioxane=10:1) and crystallization from petroleum ether

출처 및 근거

ORD 기록
ord-da5ef040252f4ae794caf6685df07b0d
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06818642B2

연결된 노트

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