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Hydrochloric Acid → HCID 49757564、化合物

HRID 600285
ノート
印刷プレビュー

反応式

HRID 600285 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH:8]C(=O)OC(C)(C)C)=[C:4]([NH:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][CH3:22])[CH:3]=1.Cl>O1CCOCC1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH2:8])=[C:4]([NH:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][CH3:22])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 45379839HCID 45379839、化合物

生成物 1

HCID 49757564HCID 49757564、化合物収率 100%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of tert-butyl 6-chloro-4-[(2-propoxyethyl)amino]pyridin-3-ylcarbamate (7.08 g, 21.4 mmol) in 1,4-dioxane (20 mL) was treated with 4N HCl in 1,4-dioxane (100 mL) and stirred at room temperature for one hour. The reaction was partitioned between ethyl acetate and saturated sodium bicarbonate solution. The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, and solvent was removed at reduced pressure to give 6-chloro-N4-(2-propoxyethyl)pyridine-3,4-diamine as a brown oil. (4.93 g, 100% yield). 1H NMR (CDCl3) δ 7.63 (1H), 6.45 (1H), 4.67 (1H), 3.67 (2H), 3.43 (2H), 3.32-3.27 (2H), 2.92 (2H), 1.64-1.55 (2H), 0.93 (3H).

後処理

  1. customThe reaction was partitioned between ethyl acetate and saturated sodium bicarbonate solution
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over magnesium sulfate, and solvent
  6. customwas removed at reduced pressure

出典と根拠

ORDレコード
ord-a39ef2b572aa47d9a8d29a14ceddee26
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902195B2

反応ノート

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