L-Tartaric acid → (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate

HRID 1653831노트

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HRID 1653831 반응식
[C:1]([OH:10])(=[O:9])[C@@H:2]([C@H:4]([C:6]([OH:8])=[O:7])[OH:5])[OH:3].[CH3:11][C@H:12]1[C:16](=[CH2:17])[CH2:15][C:14]2([CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]2)[O:13]1>C(O)C>[OH2:3].[C:6]([C@@H:4]([C@H:2]([C:1]([OH:10])=[O:9])[OH:3])[OH:5])([OH:8])=[O:7].[CH3:11][C@H:12]1[C:16](=[CH2:17])[CH2:15][C:14]2([CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]2)[O:13]1

참가 물질

4

반응물 2

HCID 444305L-Tartaric acidHCID 6918122(S)-2,8-Dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane

생성물 1

HCID 6918121(-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate수율 163.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
65 °C

실험 절차

To 28 l of 90% aqueous ethanol (water:ethanol =1:9, v/v), 7.74 kg of L-tartaric acid was added and dissolved by heating at 65° C. To the resulting solution was added 9.41 kg of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8azaspiro[4.5]decane dropwise. The mixture was allowed to cool and maintained for crystallization at 0° C. for 15 hours. The resulting crystals were collected by filtration and dried under reduced pressure to give 14.76 kg of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate. The physicochemical properties of this compound were in agreement with those of the compound obtained in Example 1.

후처리

  1. dissolutiondissolved
  2. temperatureto cool
  3. temperaturemaintained for crystallization at 0° C. for 15 hours
  4. filtrationThe resulting crystals were collected by filtration
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8832e1eaccea4b7b8650ad97c9844f74
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403931

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