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Ethyl isocyanate → HCID 59603111, 화합물

HRID 2068713
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HRID 2068713 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[N:10]=[C:9]([NH2:11])[S:8][C:5]2=[N:6][CH:7]=1.[CH2:12]([N:14]=[C:15]=[O:16])[CH3:13]>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]2[N:10]=[C:9]([NH:11][C:15]([NH:14][CH2:12][CH3:13])=[O:16])[S:8][C:5]2=[N:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 8022Ethyl isocyanateHCID 446127746-Bromo[1,3]thiazolo[5,4-b]pyridin-2-amine

생성물 1

HCID 59603111HCID 59603111, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

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온도
80 °C

실험 절차

To a solution of 6-bromothiazolo[5,4-b]pyridin-2-amine IV (1.30 g, 5.55 mmol) in 1,4-dioxane (20.0 mL) was added ethylisocyanate (2.19 mL, 27.07 mmol) and the resulting reaction mixture was heated to 80° C. for 8 h. After the completion of the reaction (TLC monitoring), 1,4-dioxane was distilled off followed by co-distillation with n-hexane (2 times). The residue was then stirred with water at 90° C. for 2 h followed by filtration to obtain the desired product that was further washed with hot water and then dried. The residue was finally washed with ether to obtain the desired product (1.40 g, 83%). 1H NMR (400 MHz, DMSO-d6): δ 1.10 (t, J=7.20 Hz, 3H), 3.20 (quintet, J=7.20 Hz, 2H), 6.76 (br s, 1H), 8.24 (d, J=2.0 Hz, 1H), 8.45 (d, J=2.0 Hz, 1H) and 11.05 (br s, 1H).

후처리

  1. customthe resulting reaction mixture
  2. distillationwas distilled off
  3. filtrationfollowed by filtration

출처 및 근거

ORD 기록
ord-bc83d38a71d24423a42a08fbac895e42
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299065B2

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