Hydrochloric Acid → 3-(1,3-Thiazol-2-yl)oxetan-3-amine hydrochloride

HRID 927725

反応式

HRID 927725 の反応式
[ClH:1].[S:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]1([NH:11]S(C(C)(C)C)=O)[CH2:10][O:9][CH2:8]1>O1CCOCC1.CO>[ClH:1].[S:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]1([NH2:11])[CH2:10][O:9][CH2:8]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 711130582-Methyl-propane-2-sulfinic acid (3-thiazol-2-yl-oxetan-3-yl)-amide

生成物 1

HCID 866747823-(1,3-Thiazol-2-yl)oxetan-3-amine hydrochloride収率 70.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

A 4.0 M solution of hydrochloric acid (117 μL, 467 μmol) in dioxane was added to a solution of 2-methyl-propane-2-sulfinic acid (3-thiazol-2-yl-oxetan-3-yl)-amide (Example 281a) (81 mg, 311 μmol) in methanol (0.5 mL) at 0° C. The mixture was stirred at 0° C. for 5 min before the solvents were removed under reduced pressure. The resulting white solid was triturated with diethyl ether and filtered off. The solid was further washed with diethyl ether and dried under high vacuum to yield the title compound (42 mg, 70%) as a white solid. MS (EI): m/e=157.1 [M+H]+.

後処理

  1. customwere removed under reduced pressure
  2. customThe resulting white solid was triturated with diethyl ether
  3. filtrationfiltered off
  4. washThe solid was further washed with diethyl ether
  5. customdried under high vacuum

出典と根拠

ORDレコード
ord-fdcf8c05978b4890bf53b9e11c3c7c63
出典データセット
uspto-grants-2016_03
特許番号
US09290451B2

関連ノート

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