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Triethylamine → 6-[(4-Tert-butylphenyl)(chloro)methyl]-3-chloro-2-methoxypyridine

HRID 70720
ノート
印刷プレビュー

反応式

HRID 70720 の反応式
S(Cl)([Cl:4])(=O)=O.[C:6]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([O:25][CH3:26])[N:19]=2)O)=[CH:12][CH:11]=1)([CH3:9])([CH3:8])[CH3:7].C(N(CC)CC)C>C1CCCCC1>[C:6]([C:10]1[CH:15]=[CH:14][C:13]([CH:16]([Cl:4])[C:18]2[N:19]=[C:20]([O:25][CH3:26])[C:21]([Cl:24])=[CH:22][CH:23]=2)=[CH:12][CH:11]=1)([CH3:9])([CH3:8])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24648Sulfuryl chlorideHCID 67396476(4-Tert-butylphenyl)(5-chloro-6-methoxypyridin-2-yl)methanol

生成物 1

HCID 673982706-[(4-Tert-butylphenyl)(chloro)methyl]-3-chloro-2-methoxypyridine収率 96%

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

Sulfuryl chloride (0.37 mL) was added to a solution of (4-tert-butylphenyl)(5-chloro-6-methoxypyridin-2-yl)methanol obtained in Example 7-4(1) (200 mg) and triethylamine (0.27 mL) in cyclohexane (4 mL) at room temperature, and then the mixture was stirred at the same temperature for 17 hours. After completion of the reaction, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1) to give 6-[(4-tert-butylphenyl)(chloro)methyl]-3-chloro-2-methoxypyridine as a colorless oil (203 mg, 96%).

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-0c602aa7de284ba0b7a9193426a57181
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822503B2

反応ノート

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