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Hydrochloric Acid → 1-Cyclopropyl-2-(5-methyl-1,3,4-oxadiazol-2-yl)propan-2-amine

HRID 1480243
ノート
印刷プレビュー

反応式

HRID 1480243 の反応式
[CH:1]1([CH2:4][C:5]([NH:13]S(C(C)(C)C)=O)([CH3:12])[C:6]2[O:7][C:8]([CH3:11])=[N:9][N:10]=2)[CH2:3][CH2:2]1.Cl.O1CCOCC1>CO>[CH:1]1([CH2:4][C:5]([C:6]2[O:7][C:8]([CH3:11])=[N:9][N:10]=2)([NH2:13])[CH3:12])[CH2:3][CH2:2]1
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 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 90203435HCID 90203435、化合物

生成物 1

HCID 902046221-Cyclopropyl-2-(5-methyl-1,3,4-oxadiazol-2-yl)propan-2-amine収率 50%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of N-[2-cyclopropyl-1-methyl-1-(5-methyl-1,3,4-oxadiazol-2-yl)ethyl]-2-methyl-propane-2-sulfinamide (example 173a, 520 mg, 1.46 mmol) in MeOH (8 ml) was added a 4M solution of hydrochloric acid in dioxane (729 μl, 2.92 mmol). The reaction mixture was stirred at room temperature for 1 hour. Reaction was quenched by addition of potassium carbonate and stirred for 15 minutes. The insolubles were removed by filtration and the filtrate was evaporated down to dryness. The crude material was purified by flash chromatography on silica eluting with a dichloromethane-methanol gradient to yield the title compound (130 mg, 50%). MS (ESI, m/z): 182.2 (M+H+).

後処理

  1. customReaction
  2. customwas quenched by addition of potassium carbonate
  3. stirringstirred for 15 minutes
  4. customThe insolubles were removed by filtration
  5. customthe filtrate was evaporated down to dryness
  6. customThe crude material was purified by flash chromatography on silica eluting with a dichloromethane-methanol gradient

出典と根拠

ORDレコード
ord-42c909ab5fa149e1a28074b79c90a81c
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409866B2

反応ノート

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