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

HRID 32800
ノート
印刷プレビュー

反応式

HRID 32800 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a57cf86785af40228e02713709f17dc7
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07427630B2

反応ノート

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