Tetrahydrofuran → HCID 59589731、化合物

HRID 1472822ノート

反応式

HRID 1472822 の反応式
O1CCCC1.[Br:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=O)[CH:15]([N:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)[CH3:16])=[CH:9][CH:8]=1>CO>[Br:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][CH2:14][CH:15]([N:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)[CH3:16])=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 8028TetrahydrofuranHCID 13221932HCID 13221932、化合物

生成物 1

HCID 59589731HCID 59589731、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 1M solution of BH3 in tetrahydrofuran (10 ml, 10 mmol) was added dropwise to N-(4-bromo-phenyl)-2-pyrrolidin-1-yl-propionamide (0.44 g, 1.48 mmol) and the solution was stirred overnight at reflux then subsequently hydrolysed by slow addition of excess of methanol and refluxing for a further 2 hours. The reaction mixture was loaded onto an SCX cartridge, which was washed with methanol and the product subsequently eluted with 2M ammonia in methanol. Removal of all solvents under rotary evaporation gave the desired product. Yield: 0.04 g, 10%. LCMS method: 2, RT: 3.07 min; MI: 283-285 [M+1].

後処理

  1. temperatureat reflux
  2. temperaturerefluxing for a further 2 hours
  3. washwas washed with methanol
  4. washthe product subsequently eluted with 2M ammonia in methanol
  5. customRemoval of all solvents
  6. customunder rotary evaporation

出典と根拠

ORDレコード
ord-bdbe0ffe3c024a9794e6f753f8b6e829
出典データセット
uspto-grants-2015_04
特許番号
US09012633B2

反応ノート

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