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

HRID 17423노트

반응식

HRID 17423 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 178502593HCID 178502593, 화합물촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-6d08f09e04354710a17d0a32a3d6a5cd
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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