3-Morpholinopropyl isothiocyanate → HCID 22118525、化合物

HRID 1274850ノート

反応式

HRID 1274850 の反応式
[Br:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][N:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)[CH2:8][CH2:9][CH2:10][NH2:11])=[CH:4][CH:3]=1.[O:20]1[CH2:25][CH2:24][N:23]([CH2:26][CH2:27][CH2:28][N:29]=[C:30]=[S:31])[CH2:22][CH2:21]1>C(Cl)(Cl)Cl.O1CCN(CCCN=C=S)CC1>[Br:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][N:7]([CH2:8][CH2:9][CH2:10][NH:11][C:30]([NH:29][CH2:28][CH2:27][CH2:26][N:23]2[CH2:24][CH2:25][O:20][CH2:21][CH2:22]2)=[S:31])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=2)=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 1417453-Morpholinopropyl isothiocyanateHCID 22118499HCID 22118499、化合物

生成物 1

HCID 22118525HCID 22118525、化合物収率 76%

試薬・触媒・溶媒 2

HCID 1417453-Morpholinopropyl isothiocyanate触媒HCID 6212Chloroform溶媒

実験手順

To a solution of N-(4-bromobenzyl)-N-(pyridin-2-yl)pro-pane-1,3-diamine (1.0 g, 3.123 mmol) in chloroform (40 ml) was added 3-morpholinopropyl isothiocyanate (593 mg, 3.123 mmol) and the reaction mixture was stirred for 20 h at reflux temperature. To the reaction mixture was added 10 drops of 3-morpholinopropyl isothiocyanate and the reaction mixture was stirred for an additional 4 h at reflux temperature. The volatiles were evaporated in vacuo and the residue (2.05 g) was dissolved in ethyl acetate (20 ml) and left over night at room temperature. The precipitate was filtered off and washed with ethyl acetate and dried affording 1.20 g (76%) of the title compound as a solid.

後処理

  1. temperatureat reflux temperature
  2. stirringthe reaction mixture was stirred for an additional 4 h
  3. temperatureat reflux temperature
  4. customThe volatiles were evaporated in vacuo
  5. dissolutionthe residue (2.05 g) was dissolved in ethyl acetate (20 ml)
  6. waitleft over night at room temperature
  7. filtrationThe precipitate was filtered off
  8. washwashed with ethyl acetate
  9. customdried

出典と根拠

ORDレコード
ord-cc944d2417724b72819436801a791e09
出典データセット
uspto-grants-2000_12
特許番号
US06159941

反応ノート

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