Carbon Tetrachloride → HCID 54218464、化合物

HRID 1863087ノート

反応式

HRID 1863087 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:21].O[CH2:26][CH2:27][CH2:28][N:29]([CH3:49])[C:30]([C:32]1[N:33]([CH3:48])[C:34]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[C:35]2[C:40]=1[CH:39]=[CH:38][C:37]([Cl:41])=[CH:36]2)=[O:31]>O1CCOCC1>[Cl:21][CH2:26][CH2:27][CH2:28][N:29]([CH3:49])[C:30]([C:32]1[N:33]([CH3:48])[C:34]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[C:35]2[C:40]=1[CH:39]=[CH:38][C:37]([Cl:41])=[CH:36]2)=[O:31]

参加物

5

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 20393369HCID 20393369、化合物

生成物 1

HCID 54218464HCID 54218464、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of 13.6 g. of triphenylphosphine in 40 ml. of carbon tetrachloride and 24 ml. of dioxane is treated with 14.3 g. of 5-chloro-2-methyl-3-phenylisoindole-1-carboxylic acid (3-hydroxypropyl)methylamide and the mixture is subsequently boiled at reflux for 1 hour. After cooling, the mixture is concentrated to dryness under reduced pressure. The residual oil is chromatographed on 800 g. of silica gel using methylene chloride/ethyl acetate (4:1) for the elution. The homogeneous fractions yield analytically pure 5-chloro-2-methyl-3-phenylisoindole-1-carboxylic acid (3-chloropropyl)methylamide as a thick yellow oil.

後処理

  1. temperatureat reflux for 1 hour
  2. temperatureAfter cooling
  3. concentrationthe mixture is concentrated to dryness under reduced pressure
  4. customThe residual oil is chromatographed on 800 g
  5. washfor the elution

出典と根拠

ORDレコード
ord-2508317066fe4edba4a26d8625f6da6a
出典データセット
uspto-grants-1979_09
特許番号
US04167632

反応ノート

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