s-1,3-Benzothiazol-2-yl benzenecarbothioate → 2,2-Bis{4-[2-benzoyloxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane

HRID 1758201

反応式

HRID 1758201 の反応式
[OH:1][CH:2]([CH2:39][N:40]1[C:49]([CH3:51])([CH3:50])[CH2:48][C:43]2([O:47][CH2:46][CH2:45][O:44]2)[CH2:42][C:41]1([CH3:53])[CH3:52])[CH2:3][O:4][CH:5]1[CH2:10][CH2:9][CH:8]([C:11]([CH:14]2[CH2:19][CH2:18][CH:17]([O:20][CH2:21][CH:22]([OH:38])[CH2:23][N:24]3[C:33]([CH3:35])([CH3:34])[CH2:32][C:27]4([O:31][CH2:30][CH2:29][O:28]4)[CH2:26][C:25]3([CH3:37])[CH3:36])[CH2:16][CH2:15]2)([CH3:13])[CH3:12])[CH2:7][CH2:6]1.[C:54](SC1SC2C=CC=CC=2N=1)(=[O:61])[C:55]1[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=1>C1C=CC=CC=1>[C:54]([O:1][CH:2]([CH2:39][N:40]1[C:41]([CH3:53])([CH3:52])[CH2:42][C:43]2([O:47][CH2:46][CH2:45][O:44]2)[CH2:48][C:49]1([CH3:51])[CH3:50])[CH2:3][O:4][CH:5]1[CH2:10][CH2:9][CH:8]([C:11]([CH:14]2[CH2:19][CH2:18][CH:17]([O:20][CH2:21][CH:22]([O:38][C:54](=[O:61])[C:55]3[CH:56]=[CH:57][CH:58]=[CH:59][CH:60]=3)[CH2:23][N:24]3[C:33]([CH3:35])([CH3:34])[CH2:32][C:27]4([O:28][CH2:29][CH2:30][O:31]4)[CH2:26][C:25]3([CH3:37])[CH3:36])[CH2:16][CH2:15]2)([CH3:12])[CH3:13])[CH2:7][CH2:6]1)(=[O:61])[C:55]1[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=1

参加物

4

反応物 2

HCID 270394s-1,3-Benzothiazol-2-yl benzenecarbothioateHCID 205106002,2-Bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane

生成物 1

HCID 205105622,2-Bis{4-[2-benzoyloxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

1.5 g of 2,2-bis{4-[2-hydroxy-3-(7,7,9,9-tetramethyl-1,4-dioxa-8-azaspiro[4.5]dec-8-yl)propoxy]cyclohexyl}propane and 1.2 g of 2-benzoylthiobenzthiazole were refluxed in 30 ml of anhydrous benzene for 4.5 hours. After completion of the reaction, the reaction mixture was treated with an aqueous alkali and then extracted with benzene, giving crystals. The crystals were purified by column chromatography through silica gel eluted with a 4:1 by volume mixture of diethyl ether and ethyl acetate. The desired Compound No. 222 was obtained in the form of a white powder melting at 77°-79° C.

後処理

  1. customAfter completion of the reaction
  2. additionthe reaction mixture was treated with an aqueous alkali and
  3. extractionthen extracted with benzene
  4. customgiving crystals
  5. customThe crystals were purified by column chromatography through silica gel
  6. washeluted with a 4:1 by volume mixture of diethyl ether and ethyl acetate

出典と根拠

ORDレコード
ord-915f9cc3d87843bab679e9efbedb4fe3
出典データセット
uspto-grants-1983_02
特許番号
US04371644

関連ノート

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