Tert-butyl 3-aminoazetidine-1-carboxylate → HCID 58777638、化合物

HRID 1371775ノート

反応式

HRID 1371775 の反応式
[NH2:1][C:2]1[C:7]([C:8]([C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[O:9])=[CH:6][N:5]=[C:4](Cl)[N:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH2:32])[CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(Cl)Cl.C(O)C>[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH:32][C:4]2[N:3]=[C:2]([NH2:1])[C:7]([C:8](=[O:9])[C:10]3[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=3[F:19])=[CH:6][N:5]=2)[CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

参加物

5

反応物 2

HCID 1516507Tert-butyl 3-aminoazetidine-1-carboxylateHCID 21070550HCID 21070550、化合物

生成物 1

HCID 58777638HCID 58777638、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

To a stirred suspension of chloropyrimidine (700 mg, 2.34 mmol, Example 289) in methylene chloride (30 mL), amine (525 mg, 5.64 mmol, Example 318) in ethanol (30 mL) was added and the mixture heated at 80° C. for 4.5 hours. The solvent was removed and the residue was dissolved in ethyl acetate and the mixture was washed successively with 0.5N hydrochloric acid and water. The organic layer was dried with sodium sulfate and concentrated to give a white solid. 1.0 g, 98%. MS (ES) MH+=436.

後処理

  1. additionwas added
  2. customThe solvent was removed
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washthe mixture was washed successively with 0.5N hydrochloric acid and water
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. concentrationconcentrated
  7. customto give a white solid

出典と根拠

ORDレコード
ord-dd962719fdbd4bd0bc96e9960a153395
出典データセット
uspto-grants-2007_01
特許番号
US07157455B2

反応ノート

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