p-Toluenesulfonic acid → HCID 178441038、化合物

HRID 2164708

反応式

HRID 2164708 の反応式
[CH2:1]([C@H:5]1[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]1)[CH2:2][CH2:3][CH3:4].C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH2:23][C:24]1([CH:49]=[CH:48][C:47]([CH2:50][CH2:51][CH2:52][CH3:53])=[CH:46][CH2:45]1)[NH:25][C:26]1[C:39]2[C:38](=[O:40])[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:31](=[O:41])[C:30]=2[CH:29]=[CH:28][C:27]=1[C:42](O)=[O:43]>ClC1C=CC=CC=1Cl>[CH2:1]([C@H:5]1[CH2:6][CH2:7][C@H:8]([O:11][C:42]([C:27]2[CH:28]=[CH:29][C:30]3[C:31](=[O:41])[C:32]4[C:37](=[CH:36][CH:35]=[CH:34][CH:33]=4)[C:38](=[O:40])[C:39]=3[C:26]=2[NH:25][C:24]2([NH2:23])[CH:45]=[CH:46][C:47]([CH2:50][CH2:51][CH2:52][CH3:53])=[CH:48][CH2:49]2)=[O:43])[CH2:9][CH2:10]1)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 704026481-Amino-4-n-butylanilinoanthraquinone-2-carboxylic acidHCID 178445814HCID 178445814、化合物

生成物 1

HCID 178441038HCID 178441038、化合物収率 46.4%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

To 200 ml of orthodichlorobenzene were added 31.6 g of trans-4-n-butylcyclohexanol, 5.6 g of p-toluenesulfonic acid, and 28 g of 1-amino-4-n-butylanilinoanthraquinone-2-carboxylic acid. The mixture was heated slowly to 110° to 115° C. and maintained at this temperature for 17 hours with stirring. The orthochlorobenzene solution was concentrated to 70 ml under reduced pressure, and 1500 ml of methanol was added. The resulting precipitates was filtered out and then purified by column chromatography wherein silica gel was used as a carrier and chloroform was used as a solvent to obtain 17.3 g of 1-amino-4-n-butylanilinoanthraquinone-2-carboxylic acid-trans-4-n-butylcyclohexyl ester.

後処理

  1. temperatureThe mixture was heated slowly to 110° to 115° C.
  2. temperaturemaintained at this temperature for 17 hours
  3. concentrationThe orthochlorobenzene solution was concentrated to 70 ml under reduced pressure, and 1500 ml of methanol
  4. additionwas added
  5. customThe resulting precipitates
  6. filtrationwas filtered out
  7. custompurified by column chromatography wherein silica gel

出典と根拠

ORDレコード
ord-c59d58e7bcc341988eed93288b59ff2a
出典データセット
uspto-grants-1985_03
特許番号
US04507221

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