2-Chloroethyl isocyanate → N-(6-Bromo-2-pyridinyl)-N'-(2-chloroethyl)urea

HRID 32800

반응식

HRID 32800 반응식
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.[Cl:9][CH2:10][CH2:11][N:12]=[C:13]=[O:14]>C1COCC1>[Br:1][C:2]1[N:7]=[C:6]([NH:8][C:13]([NH:12][CH2:11][CH2:10][Cl:9])=[O:14])[CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 160352-Chloroethyl isocyanateHCID 3008092-Amino-6-bromopyridine

생성물 1

HCID 58791151N-(6-Bromo-2-pyridinyl)-N'-(2-chloroethyl)urea수율 66%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 6-bromo-2-pyridinamine (1 g, 5.78 mmol) in anh. THF (25 mL), at r.t., under N2, was added 1-chloro-2-isocyanatoethane (1.2 mL, 2.5 eq) and the reaction mixture was stirred at r.t. for 18 hr. The crude mixture was partitioned between CH2Cl2 and water. The phases were separated and the organic layer was dried over anh. Na2SO4. The solids were filtered and the solvent evaporated to give the title compound (1.06 g, 66%) which was used in the next step without further purification.

후처리

  1. customThe crude mixture was partitioned between CH2Cl2 and water
  2. customThe phases were separated
  3. dry with materialthe organic layer was dried over anh. Na2SO4
  4. filtrationThe solids were filtered
  5. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-a57cf86785af40228e02713709f17dc7
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07427630B2

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