Water → HCID 46945368、化合物

HRID 2370597ノート

反応式

HRID 2370597 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([CH3:15])([CH3:14])[N:10]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25][CH2:26][CH2:27][CH2:28][C:29]([F:35])([F:34])[C:30]([F:33])([F:32])[F:31])[C:9]2=[O:36])=[CH:4][C:3]=1[CH3:37].[CH:38]([N:42]=[C:43]=[O:44])([CH2:40][CH3:41])[CH3:39].O>ClCCCl>[CH3:14][C:11]1([CH3:15])[C:12](=[O:13])[N:8]([C:5]2[CH:6]=[CH:7][C:2]([NH:1][C:43]([NH:42][CH:38]([CH3:39])[CH2:40][CH3:41])=[O:44])=[C:3]([CH3:37])[CH:4]=2)[C:9](=[O:36])[N:10]1[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25][CH2:26][CH2:27][CH2:28][C:29]([F:35])([F:34])[C:30]([F:33])([F:31])[F:32]

参加物

5

反応物 3

HCID 962WaterHCID 5508502-IsocyanatobutaneHCID 46945366HCID 46945366、化合物

生成物 1

HCID 46945368HCID 46945368、化合物収率 36%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

The compound of Example 25 (395 mg, 0.72 mmole) is dissolved in anhydrous 1,2-dichloroethane (10 ml) under an argon atmosphere, before the dropwise addition of sec-butylisocyanate (0.35 ml, 3 mmoles) at 23° C. The mixture is then heated under reflux for 24 hours. The reaction medium is then poured onto cold water and extracted using CH2Cl2. After decantation, the organic phase is washed with water and salt water. The organic solution is then dried over MgSO4, filtered, concentrated to dryness under vacuum and the evaporation residue is purified on a silica column (eluent: heptane/AcOEt: 1/0 to 4/6). The expected compound is obtained in the form of a colourless oil with a yield of 36%.

後処理

  1. temperatureThe mixture is then heated
  2. temperatureunder reflux for 24 hours
  3. extractionextracted
  4. washAfter decantation, the organic phase is washed with water and salt water
  5. dry with materialThe organic solution is then dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under vacuum
  8. customthe evaporation residue is purified on a silica column (eluent: heptane/AcOEt: 1/0 to 4/6)

出典と根拠

ORDレコード
ord-618c4242463042b18fcf5676750282e1
出典データセット
uspto-grants-2014_04
特許番号
US08710091B2

反応ノート

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