Morpholine → 4-(Morpholin-4-ylmethyl)-1,3-thiazol-2-amine

HRID 1684947

반응식

HRID 1684947 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl.Cl[CH2:9][C:10]1[N:11]=[C:12]([NH2:15])[S:13][CH:14]=1>CN(C=O)C.C(OCC)(=O)C>[O:4]1[CH2:5][CH2:6][N:1]([CH2:9][C:10]2[N:11]=[C:12]([NH2:15])[S:13][CH:14]=2)[CH2:2][CH2:3]1

참가 물질

5

반응물 2

HCID 8083MorpholineHCID 732282-Thiazolamine, 4-(chloromethyl)-, hydrochloride (1:1)

생성물 1

HCID 21253444-(Morpholin-4-ylmethyl)-1,3-thiazol-2-amine

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

Morpholine (350 μL, 4.0.0 mmol) is added to a solution of 4-chloromethyl-thiazol-2-ylamine hydrochloride (368 mg, 2.00 mmol) in DMF (7 mL). The reaction is stirred at 90° C. for 16 h. The reaction is diluted with ethyl acetate and washed with water. The aqueous layer is concentrated in vacuo and extracted with ethyl acetate. The combined organic layers are dried over MgSO4 and evaporated to give brown crystals which are used without further purification. 1H-NMR (400 MHz, d6-DMSO) δ=2.41-2.42 (m, 4H, CH2CH2), 3.30 (s, 2H, CH2), 3.55-3.60 (m, 4H, CH2CH2), 6.33 (s, 1H, Har), 6.85 (bs, 2H, NH2).

후처리

  1. washwashed with water
  2. concentrationThe aqueous layer is concentrated in vacuo
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic layers are dried over MgSO4
  5. customevaporated
  6. customto give brown crystals which
  7. customare used without further purification

출처 및 근거

ORD 기록
ord-f5185dbf08d14591b0c720c939f657fc
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148369B2

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