Water → HCID 86723563、化合物

HRID 2201657ノート

反応式

HRID 2201657 の反応式
[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH2:7])[CH2:3]1.C([O-])([O-])=O.[Na+].[Na+].Cl[C:15]([O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:16].O>O1CCCC1>[CH2:1]=[C:2]1[CH2:5][CH:4]([CH2:6][NH:7][C:15](=[O:16])[O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:3]1

参加物

6

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10387Benzyl chloroformateHCID 177500821-(3-Methylidenecyclobutyl)methanamine

生成物 1

HCID 86723563HCID 86723563、化合物収率 56.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 4-2 (3 g, 30.9 mmol) was dissolved in 50 mL of tetrahydrofuran, added Na2CO3 (6.3 g, 60 mmol) and benzyl chloroformate (5.25 g, 30.8 mmol). The mixture was stirred for 12 hours at room temperature, added 100 mL of water, extracted three times with 300 mL of ethyl acetate, combined the organic phases, rotary evaporated to remove solvents and purified by column chromatography (petroleum ether/ethyl acetate=10:1) to give Compound 4-3 (4 g, 56% yield).

後処理

  1. extractionextracted three times with 300 mL of ethyl acetate
  2. customrotary evaporated
  3. customto remove solvents
  4. custompurified by column chromatography (petroleum ether/ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-eef0e8133ab7412380e1dd79abf4ccb8
出典データセット
uspto-grants-2016_06
特許番号
US09365499B2

反応ノート

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