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

반응식

HRID 1758201 반응식
[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

참가 물질

4

반응물 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

생성물 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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-915f9cc3d87843bab679e9efbedb4fe3
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04371644

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