Acetyl chloride → HCID 58997658、化合物

HRID 1592353

反応式

HRID 1592353 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][NH2:11])=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:21])[CH3:20]>C1COCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][NH:11][C:19](=[O:21])[CH3:20])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 64837963-(4-Fluorophenyl)propan-1-amine

生成物 1

HCID 58997658HCID 58997658、化合物収率 86.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1-(para-fluorophenyl)-3-aminopropane (1.00 g, 6.53 mmol, 1 eq.) and triethylamine (0.91 mL, 6.53 mmol, 1 eq.) were dissoved in THF (10 mL) at 25° C. under N2. Then a THF solution (5 mL) of acetyl chloride (0.46 mL, 6.53 mmol, 1 eq.) was added dropwise via an addition funnel over 10 minutes. Worked up after 20 minutes by filtering off the solids then stripping the filtrate to obtain an amber oil. The oil was purified over silica gel in 1:1 Hexanes/EtOAc to 100% EtOAc to 4:1 EtOAc/MeOH. Obtained 1.10 g of an amber oil as product. MS (ESI) detects (M+H)+=196.

後処理

  1. filtrationby filtering off the solids
  2. customto obtain an amber oil
  3. customThe oil was purified over silica gel in 1:1 Hexanes/EtOAc to 100% EtOAc to 4:1 EtOAc/MeOH

出典と根拠

ORDレコード
ord-97594fdb46f9489b82ad8fee77b8bec0
出典データセット
uspto-grants-2007_11
特許番号
US07291744B2

関連ノート

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