HCID 86702385、化合物 → HCID 86702386、化合物

HRID 1851245ノート

反応式

HRID 1851245 の反応式
[NH2:1][C:2]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[N:19]=1)=[N:3][NH:4][C:5]([CH:7]1[CH2:10][N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:8]1)=O>C(O)C>[CH3:24][C:20]1[N:19]=[C:18]([C:2]2[N:1]=[C:5]([CH:7]3[CH2:10][N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:8]3)[NH:4][N:3]=2)[CH:23]=[CH:22][CH:21]=1

参加物

3

反応物 1

HCID 86702385HCID 86702385、化合物

生成物 1

HCID 86702386HCID 86702386、化合物収率 83%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

16.4 g (49.3 mmol) tert-Butyl 3-({2-[amino(6-methylpyridine-2-yl)methylene]hydrazino}carbonyl)azetidine-1-carboxylate are heated under a nitrogen atmosphere to the melting point (220° C.) and kept there for 90 minutes. Ethanol is cautiously added to the reaction mixture during the cooling down phase (at around 135° C.). The reaction mixture is stirred over night at room temperature and the ethanol is evaporated. Due to an incomplete reaction the residue is heated once more to 220° C. for one hour and the work up is repeated yielding 12.91 g (74.58%) of the desired crude product (the byproduct is the cyclised compound which has lost the Boc group).

後処理

  1. customthe ethanol is evaporated
  2. customDue to an incomplete reaction the residue
  3. temperatureis heated once more to 220° C. for one hour

出典と根拠

ORDレコード
ord-e2320281abda4a90afe668ffba273b47
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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