HCID 86750864, 화합물 → HCID 22872811, 화합물

HRID 1780969노트

반응식

HRID 1780969 반응식
[C:1]1([C:7]2([C:43]3[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=3)[C@H:15]3[C@H:11]([CH2:12][N:13]([C:16](=[O:32])[CH2:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[O:24]CC4C=CC=CC=4)[CH2:14]3)[C@:10]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[O:40][CH3:41])([OH:33])[CH:9]([OH:42])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1>[OH-].[OH-].[Pd+2].C(O)C>[C:43]1([C:7]2([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C@H:15]3[C@H:11]([CH2:12][N:13]([C:16](=[O:32])[CH2:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[OH:24])[CH2:14]3)[C@:10]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[O:40][CH3:41])([OH:33])[C@H:9]([OH:42])[CH2:8]2)[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1

참가 물질

4

반응물 1

HCID 86750864HCID 86750864, 화합물

생성물 1

HCID 22872811HCID 22872811, 화합물수율 84.6%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

A mixture of 1.5 g of (3aR,4R, SR,7aR)-7,7-diphenyl-4-(2-methoxyphenyl)-2-[(2-benzyloxyphenyl)acetyl]perhydro-4,5-isoindolediol and 50 cm3 of ethanol is heated to 60° C. with stirring; 0.5 g of 20% palladium hydroxide on charcoal is added and the reaction mixture is then hydrogenated, with stirring, at a temperature of 60° C. and at atmospheric pressure. After reaction for 45 minutes, the theoretical volume of hydrogen has been absorbed; the reaction mixture is filtered, followed by concentration to dryness under reduced pressure (2.7 kPa). The meringue-like product obtained is purified by crystallization in 10 cm3 of isopropyl ether to give 1.09 g of (3aR,4R,5R,7aR)-7,7-diphenyl-4-(2-methoxyphenyl)-2-[(2-hydroxyphenyl)acetyl]perhydro-4,5-isoindolediol, melting at 188° C.

후처리

  1. stirringhydrogenated, with stirring, at a temperature of 60° C. and at atmospheric pressure
  2. customAfter reaction for 45 minutes
  3. customthe theoretical volume of hydrogen has been absorbed
  4. filtrationthe reaction mixture is filtered
  5. concentrationfollowed by concentration to dryness under reduced pressure (2.7 kPa)
  6. customThe meringue-like product obtained
  7. customis purified by crystallization in 10 cm3 of isopropyl ether

출처 및 근거

ORD 기록
ord-50951ff0bd514fd4ae9a987c41fc417e
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05631279

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