Formic Acid → 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-1-methyl-4-phenylazepane

HRID 11219

反応式

HRID 11219 の反応式
[F:1][C:2]([F:30])([F:29])[C:3]1[CH:4]=[C:5]([CH:22]=[C:23]([C:25]([F:28])([F:27])[F:26])[CH:24]=1)[CH2:6][O:7][CH2:8][C:9]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:15][CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.C=O.[CH:33](O)=O>C(Cl)(Cl)Cl>[F:30][C:2]([F:29])([F:1])[C:3]1[CH:4]=[C:5]([CH:22]=[C:23]([C:25]([F:28])([F:27])[F:26])[CH:24]=1)[CH2:6][O:7][CH2:8][C:9]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:15][CH2:14][CH2:13][N:12]([CH3:33])[CH2:11][CH2:10]1

参加物

5

反応物 3

HCID 284Formic AcidHCID 712FormaldehydeHCID 116261604-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane

生成物 1

HCID 219731264-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-1-methyl-4-phenylazepane収率 67%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
65 °C

実験手順

The mixture of Isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane (3 mg), paraformaldehyde (3 mg) and formic acid (2.2 mg) in chloroform (0.1 mL) was stirred at 65° C. for overnight. After cooling down, the mixture was concentrated under vacuum and filtered through anion exchange cartridge to get rid of formic acid. The crude product was purified by prep TLC with 10% methanol/89% dichloromethane/1% NH4OH to give the product as a clear sticky oil (2 mg, 67% yield).

後処理

  1. temperatureAfter cooling down
  2. concentrationthe mixture was concentrated under vacuum
  3. filtrationfiltered through anion exchange cartridge
  4. customto get rid of formic acid
  5. customThe crude product was purified by prep TLC with 10% methanol/89% dichloromethane/1% NH4OH

出典と根拠

ORDレコード
ord-7c45a7a9c1bb48d9913c24128571cdaf
出典データセット
uspto-grants-2006_08
特許番号
US07098203B2

関連ノート

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