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Triethylamine → [(2-Chloroethyl)amino]-n-(4-fluoroindanyl)carboxamide

HRID 1924841
ノート
印刷プレビュー

反応式

HRID 1924841 の反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2[NH2:11].C(N(CC)CC)C.[Cl:19][CH2:20][CH2:21][N:22]=[C:23]=[O:24]>C(Cl)Cl>[Cl:19][CH2:20][CH2:21][NH:22][C:23]([NH:11][CH:6]1[C:7]2[C:3](=[C:2]([F:1])[CH:10]=[CH:9][CH:8]=2)[CH2:4][CH2:5]1)=[O:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 160352-Chloroethyl isocyanateHCID 162443184-fluoro-2,3-dihydro-1H-inden-1-amine

生成物 1

HCID 59355772[(2-Chloroethyl)amino]-n-(4-fluoroindanyl)carboxamide収率 33.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred, cold (0° C.) solution of 7.0 grams (0.046 mole) of 4-fluoroindanylamine (known compound) and 5.7 grams (0.056 mole) of triethylamine in 100 mL of methylene chloride was added 5.4 grams (0.051 mole) of 2-chloroethyl isocyanate. The cold reaction mixture was stirred for three hours at which time it was filtered. The filter cake was rinsed with methylene chloride. The filtrates were combined and concentrated under reduced pressure to a residue. The residue was triturated with hexanes and the mixture filtered. The filter cake was dried under reduced pressure to yield 4.0 grams of [(2-chloroethyl)amino]-N-(4-fluoroindanyl)carboxamide. The NMR spectrum was consistent with the proposed structure.

後処理

  1. customThe cold reaction mixture
  2. filtrationwas filtered
  3. washThe filter cake was rinsed with methylene chloride
  4. concentrationconcentrated under reduced pressure to a residue
  5. customThe residue was triturated with hexanes
  6. filtrationthe mixture filtered
  7. customThe filter cake was dried under reduced pressure

出典と根拠

ORDレコード
ord-1646a22f78fb499d8946714d0c3cae23
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08178567B2

反応ノート

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