Acetyl chloride → tert-Butyl (1-acetylazetidin-3-yl)(methyl)carbamate

HRID 17423ノート

反応式

HRID 17423 の反応式
[CH:1]([N:14]1[CH2:17][CH:16]([N:18]([CH3:26])[C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:15]1)(C1C=CC=CC=1)[C:2]1C=CC=CC=1.C(N(CC)CC)C.C(Cl)(=[O:36])C>[OH-].[Pd+2].[OH-].[C].CO>[C:1]([N:14]1[CH2:17][CH:16]([N:18]([CH3:26])[C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH2:15]1)(=[O:36])[CH3:2]

参加物

6

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 53446336tert-Butyl (1-benzhydrylazetidin-3-yl)(methyl)carbamate

生成物 1

HCID 86630849tert-Butyl (1-acetylazetidin-3-yl)(methyl)carbamate

試薬・触媒・溶媒 2

HCID 178502593HCID 178502593、化合物触媒HCID 887Methanol溶媒

実験手順

tert-Butyl N-(1-benzhydrylazetidin-3-yl)-N-methylcarbamate (I-149) (0.40 g, 1.13 mmol) was dissolved methanol (20 ml), then 20% palladium hydroxide-carbon (containing about 50% water, 20 g) was added, followed by stirring at room temperature under hydrogen atmosphere for 15 hours, and the catalyst was removed by filtration. The solvent was evaporated away under reduced pressure, the resulting residue was dissolved in dichloromethane (10 ml), and triethylamine (0.20 ml, 3.44 mmol) and acetyl chloride (90.0 μl, 26 mmol) were added.

後処理

  1. customthe catalyst was removed by filtration
  2. customThe solvent was evaporated away under reduced pressure
  3. dissolutionthe resulting residue was dissolved in dichloromethane (10 ml)

出典と根拠

ORDレコード
ord-6d08f09e04354710a17d0a32a3d6a5cd
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

反応ノート

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