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Hydrochloric Acid → HCID 46897236、化合物

HRID 1966966
ノート
印刷プレビュー

反応式

HRID 1966966 の反応式
C(N(CC)C(C)C)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[O:32]=[C:33]1[N:37]([CH2:38][C:39]([OH:41])=O)[C:36](=[O:42])[C:35]2([CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)[N:34]1[C:48]1[CH:53]=[CH:52][C:51]([CH3:54])=[CH:50][CH:49]=1.[C:55]1([CH:61]([NH2:65])[CH2:62][CH2:63][CH3:64])[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=1.Cl>CN1C(=O)CCC1>[O:32]=[C:33]1[N:37]([CH2:38][C:39]([NH:65][CH:61]([C:55]2[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=2)[CH2:62][CH2:63][CH3:64])=[O:41])[C:36](=[O:42])[C:35]2([CH2:47][CH2:46][CH2:45][CH2:44][CH2:43]2)[N:34]1[C:48]1[CH:53]=[CH:52][C:51]([CH3:54])=[CH:50][CH:49]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 36037851-Phenylbutan-1-amine2 回HCID 66680556HCID 66680556、化合物

生成物 1

HCID 46897236HCID 46897236、化合物

試薬・触媒・溶媒

1
HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

170 μl (0.098 mmol, 0.1 eq.) of N,N-diisopropylethylamine and 204 mg (0.63 mmol, 2 eq.) of TBTU are added to a solution of 100 mg of (2,4-dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)acetic acid in 30 ml of NMP. The solution is stirred for 20 minutes, and 70 mg (0.47 mmol, 1.5 eq.) of 1-phenylbutylamine (starting material 3) are added. The reaction medium is stirred overnight at room temperature. It is then poured into 1N hydrochloric acid solution and extracted with ethyl acetate. The organic phase is then washed with water, then with 1N sodium hydroxide solution, and then again with water. It is dried over sodium sulfate. The residue is precipitated from dichloromethane and heptane. 2-(2,4-Dioxo-1-p-tolyl-1,3-diazaspiro[4.5]dec-3-yl)-N-(1-phenylbutyl)acetamide is obtained in the form of a white solid.

後処理

  1. stirringThe reaction medium is stirred overnight at room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is then washed with water
  4. dry with materialIt is dried over sodium sulfate
  5. customThe residue is precipitated from dichloromethane and heptane

出典と根拠

ORDレコード
ord-5e277f2a924d49a2b2c3c94c58edaf87
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08420681B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート