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

HRID 927725

반응식

HRID 927725 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

반응 조건

온도
0 °C

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-fdcf8c05978b4890bf53b9e11c3c7c63
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290451B2

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