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1-(4-Hydroxynaphthalen-1-yl)thiolan-1-ium chloride → HCID 86662326、化合物

HRID 2405631
ノート
印刷プレビュー

反応式

HRID 2405631 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

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

生成物 1

HCID 86662326HCID 86662326、化合物収率 43%

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-f3337d57a91143e79c79a75604258d92
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08808964B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート