Water → 2-(3-Methyl-1,2,4-thiadiazol-5-yl)propan-2-amine

HRID 631990ノート

反応式

HRID 631990 の反応式
[CH3:1][C:2]1[N:6]=[C:5]([C:7]([NH:10]C(=O)OC(C)(C)C)([CH3:9])[CH3:8])[S:4][N:3]=1.O>Cl.C(OCC)(=O)C>[CH3:8][C:7]([NH2:10])([C:5]1[S:4][N:3]=[C:2]([CH3:1])[N:6]=1)[CH3:9]

参加物

5

反応物 2

HCID 962WaterHCID 71087465HCID 71087465、化合物

生成物 1

HCID 866747402-(3-Methyl-1,2,4-thiadiazol-5-yl)propan-2-amine収率 87.7%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of tert-butyl 2-(3-methyl-1,2,4-thiadiazol-5-yl)propan-2-ylcarbamate (0.15 g, 0.58 mmol) in saturated hydrochloride in ethyl acetate (10 mL) was stirred at room temperature for 1 h. Then water (20 mL) was added. The water phase was washed with ethyl acetate (2×20 mL). Then the water phase was adjusted with sodium hydroxide solution (2 M) to pH=9˜10 and extracted with ethyl acetate (3×20 mL). The combined organic layer was washed with brine (20 mL), dried over anhydrous sodium sulfate and concentrated to give product (0.08 g, 87%) as yellow oil; MS (EI): m/e 231.1 [M+H]+.

後処理

  1. washThe water phase was washed with ethyl acetate (2×20 mL)
  2. extractionextracted with ethyl acetate (3×20 mL)
  3. washThe combined organic layer was washed with brine (20 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-f2840fc40c934990aa913378cd58b924
出典データセット
uspto-grants-2016_04
特許番号
US09321727B2

反応ノート

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