Triethylamine → 1-Benzhydryl-N-methylazetidine-3-carboxamide

HRID 868116ノート

反応式

HRID 868116 の反応式
[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:8]2[CH2:11][CH:10]([C:12](O)=[O:13])[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21](N1C=CN=C1)([N:23]1C=CN=C1)=O.C(N(CC)CC)C.Cl.CN>C(#N)C>[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:8]2[CH2:11][CH:10]([C:12]([NH:23][CH3:21])=[O:13])[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 27354401-(Diphenylmethyl)azetidine-3-carboxylic acidHCID 6364545Methylamine hydrochloride

生成物 1

HCID 137728491-Benzhydryl-N-methylazetidine-3-carboxamide収率 114.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

To a solution of 7.5 g (28 mmole) of 1-(diphenylmethyl)azetidine-3-carboxylic acid in 75 ml of acetonitrile was added 6.0 g (37 mmole) of 1,1'-carbonyldiimidazole. The reaction was heated at 60° C. for two hours and successively treated with 3.11 g (30.8 mmole) of triethylamine and 2.08 g (30.8 mmole) of methylamine hydrochloride. The reaction was stirred at 60° C. for an additional hour, the solvent evaporated in vacuo, and the residue dissolved in chloroform. After washing with water and drying over magnesium sulfate, the chloroform layer was evaporated in vacuo to give 9.0 g of 1-(diphenylmethyl)-N-methyl-3-azetidinecarboxamide, mp 103°-107° C.

後処理

  1. customthe solvent evaporated in vacuo
  2. dissolutionthe residue dissolved in chloroform
  3. washAfter washing with water
  4. dry with materialdrying over magnesium sulfate
  5. customthe chloroform layer was evaporated in vacuo

出典と根拠

ORDレコード
ord-eb4c3939f6e24da6abac1852b52814dd
出典データセット
uspto-grants-1988_10
特許番号
US04777175

反応ノート

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