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Triethylamine → 3-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]-benzamido}-5-butanoyloxy-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-1H-pyrazole

HRID 1660540
ノート
印刷プレビュー

反応式

HRID 1660540 の反応式
[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:50])[CH3:49])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[CH:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)[C:22](=[O:29])[N:21]([C:30]2[C:35]([Cl:36])=[CH:34][C:33]([Cl:37])=[CH:32][C:31]=2[Cl:38])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.[C:60](OCl)(=[O:64])[CH2:61][CH2:62][CH3:63].C(OCC)(=O)C>O1CCCC1>[C:1]([C:6]1[CH:47]=[C:46]([C:48]([CH2:51][CH3:52])([CH3:49])[CH3:50])[CH:45]=[CH:44][C:7]=1[O:8][CH:9]([CH2:42][CH3:43])[C:10]([NH:12][C:13]1[CH:14]=[C:15]([CH:39]=[CH:40][CH:41]=1)[C:16]([NH:18][C:19]1[C:23]([N:24]2[CH:28]=[CH:27][CH:26]=[N:25]2)=[C:22]([O:29][C:60](=[O:64])[CH2:61][CH2:62][CH3:63])[N:21]([C:30]2[C:31]([Cl:38])=[CH:32][C:33]([Cl:37])=[CH:34][C:35]=2[Cl:36])[N:20]=1)=[O:17])=[O:11])([CH2:4][CH3:5])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 136682733-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]benzamido}-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-5-oxo-2-pyrazolineHCID 18444075Butanoyloxy chloride

生成物 1

HCID 205569513-{3-[2-(2,4-Di-tert-amylphenoxy)butyramido]-benzamido}-5-butanoyloxy-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-1H-pyrazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

30.6 g of 3-{3-[2-(2,4-di-tert-amylphenoxy)butyramido]benzamido}-1-(2,4,6-trichlorophenyl)-4-(1-pyrazolyl)-5-oxo-2-pyrazoline (prepared by the method described in German Patent Application (OLS) No. 2,536,191) was dissolved in 100 ml of tetrahydrofuran and 5 g of triethylamine was added. To the solution, a solution containing 3.5 g of butanoyloxy chloride dissolved in 10 ml of tetrahydrofuran was dropwise added. After the addition of the solution, the mixture was stirred for 1 hour. 500 ml of ethyl acetate was added to the reaction mixture and washed several times with water. The oil layer was dried with anhydrous sodium sulfate and concentrated. Upon crystallization of the residue from acetonitrile, 24 g of Coupler (5) was obtained. The melting point of the coupler was 63° to 68° C.

後処理

  1. additionwas dropwise added
  2. additionAfter the addition of the solution
  3. washwashed several times with water
  4. dry with materialThe oil layer was dried with anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customUpon crystallization of the residue from acetonitrile, 24 g of Coupler (5)
  7. customwas obtained
  8. customwas 63° to 68° C.

出典と根拠

ORDレコード
ord-b3fad9f1cffc42d2ba9d9de60a7fb7f4
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04308343

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