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1-(4-Hydroxynaphthalen-1-yl)thiolan-1-ium chloride → HCID 86662326, 화합물

HRID 1622059
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HRID 1622059 반응식
[F:1][C:2]([F:25])([S:21]([O-:24])(=[O:23])=[O:22])[CH:3]([O:8][C:9]([C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][CH:13]([CH2:14]3)[CH2:12]1)[CH2:18]2)=[O:10])[C:4]([F:7])([F:6])[F:5].[Na+].[Cl-].[OH:28][C:29]1[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:32]([S+:39]2[CH2:43][CH2:42][CH2:41][CH2:40]2)=[CH:31][CH:30]=1>>[C:11]12([C:9]([O:8][CH:3]([C:4]([F:7])([F:5])[F:6])[C:2]([F:1])([F:25])[S:21]([O-:24])(=[O:22])=[O:23])=[O:10])[CH2:12][CH:13]3[CH2:19][CH:17]([CH2:16][CH:15]([CH2:14]3)[CH2:20]1)[CH2:18]2.[OH:28][C:29]1[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:32]([S+:39]2[CH2:40][CH2:41][CH2:42][CH2:43]2)=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 714422161-(4-Hydroxynaphthalen-1-yl)thiolan-1-ium chlorideHCID 86662327Sodium 1,1,3,3,3-pentafluoro-2-(adamantane-1-carbonyloxy)propanesulfonate

생성물 1

HCID 86662326HCID 86662326, 화합물수율 43%

실험 절차

An aqueous solution of sodium 1,1,3,3,3-pentafluoro-2-(adamantane-1-carbonyloxy)propanesulfonate (corresponding to 0.021 mol) synthesized according to the formulation described in JP-A 2007-145797 was mixed with the aqueous solution of 4-hydroxynaphthyl-1-tetrahydrothiophenium chloride (corresponding to 0.023 mol) synthesized in Reference Synthesis Example 1. The mixture was extracted with 100 g of dichloromethane and 50 g of methyl isobutyl ketone. The organic layer was washed with water, and the solvent was distilled off in vacuum. The residue was poured into isopropyl ether for crystallization, filtered and dried, obtaining the target compound. White crystal, 6.2 g, yield 43%.

후처리

  1. customsynthesized in Reference Synthesis Example 1
  2. extractionThe mixture was extracted with 100 g of dichloromethane and 50 g of methyl isobutyl ketone
  3. washThe organic layer was washed with water
  4. distillationthe solvent was distilled off in vacuum
  5. additionThe residue was poured into isopropyl ether for crystallization
  6. filtrationfiltered
  7. customdried
  8. customobtaining the target compound

출처 및 근거

ORD 기록
ord-1f644e01b03f44048e8230065b47b649
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778591B2

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