1-Boc-Azetidine-3-carboxylic acid → HCID 86702385、化合物

HRID 1851244ノート

反応式

HRID 1851244 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:11][CH:10]([C:12]([OH:14])=O)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(C1NC=CN=1)(C1NC=CN=1)=O.[CH3:27][C:28]1[N:33]=[C:32]([C:34](=[N:36][NH2:37])[NH2:35])[CH:31]=[CH:30][CH:29]=1>ClCCl>[NH2:35][C:34]([C:32]1[CH:31]=[CH:30][CH:29]=[C:28]([CH3:27])[N:33]=1)=[N:36][NH:37][C:12]([CH:10]1[CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:11]1)=[O:14]

参加物

5

反応物 3

HCID 27559811-Boc-Azetidine-3-carboxylic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 573576606-Methylpicolinimidohydrazide

生成物 1

HCID 86702385HCID 86702385、化合物収率 90.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 8.21 g (54.7 mmol) 1-(tert-butoxycarbonyl) azetidine-3-carboxylic acid in 80 mL dichloromethane are added 8.86 g (54.7 mmol) carbonyl diimidazole within 30 min. After stirring for five minutes 11 g (54.7 mmol) 6-methylpyridine-2-carbohydrazonamide are added and the reaction mixture is stirred at room temperature for 3 hours. The solvent has been evaporated and the residue is treated with water. The formed precipitate has been filtered off and dried yielding 16.47 g (81.3%) of the desired compound as a mixture of tautomers.

後処理

  1. additionare added
  2. customThe solvent has been evaporated
  3. additionthe residue is treated with water
  4. filtrationThe formed precipitate has been filtered off
  5. customdried

出典と根拠

ORDレコード
ord-06f3c10fbcd84ab89b644dd99746e39a
出典データセット
uspto-grants-2015_02
特許番号
US08957064B2

反応ノート

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