Carbon tetrabromide → HCID 60209911、化合物

HRID 1433100ノート

反応式

HRID 1433100 の反応式
O[CH2:2][C:3]1[CH:4]=[N:5][C:6]([S:9][CH3:10])=[N:7][CH:8]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:31]>C1C=CC=CC=1>[Br:31][CH2:2][C:3]1[CH:4]=[N:5][C:6]([S:9][CH3:10])=[N:7][CH:8]=1

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 22050485(2-(Methylsulfanyl)pyrimidin-5-yl)methanol

生成物 1

HCID 60209911HCID 60209911、化合物収率 61%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

5-hydroxymethyl-2-methylthiopyrimidine (0.1 g, 0.61 mmol), triphenylphosphine (0.45 g, 1.7 mmol) and carbon tetrabromide (0.28 g, 0.85 mmol) are stirred in benzene (5 mL) for 24 h. The mixture is evaporated and the residue is purified by flash chromatography (silica gel, 4:1 hexanes/ethyl acetate) to provide the intermediate title compound as a white solid (0.08 g, 61%). MS (ES), 219/221 [M+H]+ (Br).

後処理

  1. customThe mixture is evaporated
  2. customthe residue is purified by flash chromatography (silica gel, 4:1 hexanes/ethyl acetate)

出典と根拠

ORDレコード
ord-e5c24fd45b004b6bb157294d4c716446
出典データセット
uspto-grants-2009_11
特許番号
US07612075B2

反応ノート

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