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Hydrochloric Acid → HCID 513971、化合物

HRID 987973
ノート
印刷プレビュー

反応式

HRID 987973 の反応式
C(OC(=O)[NH:7][C@H:8]([C:20](=[O:44])[NH:21][CH2:22][CH2:23][CH2:24][CH2:25][C@H:26]([N:29]([S:34]([C:37]1[CH:42]=[CH:41][C:40]([NH2:43])=[CH:39][CH:38]=1)(=[O:36])=[O:35])[CH2:30][CH:31]([CH3:33])[CH3:32])[CH2:27][OH:28])[CH2:9][C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=1)(C)(C)C.Cl>C(O)C>[NH2:7][C@@H:8]([CH2:9][C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=1)[C:20]([NH:21][CH2:22][CH2:23][CH2:24][CH2:25][C@H:26]([N:29]([S:34]([C:37]1[CH:38]=[CH:39][C:40]([NH2:43])=[CH:41][CH:42]=1)(=[O:36])=[O:35])[CH2:30][CH:31]([CH3:33])[CH3:32])[CH2:27][OH:28])=[O:44]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59100715HCID 59100715、化合物

生成物 1

HCID 513971HCID 513971、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(1S,5S)-(1-{5-[(4-amino-benzenesulfonyl)-isobutyl-amino]-6-hydroxy-hexylcarbamoyl}-2-naphthalen-2-yl-ethyl)-carbamic acid tert-butyl ester (698 mg, 1.089 mmol) was added to 6 mL of ethanol and 6 mL of HCl. The mixture was stirred at room temperature until completion by TLC. The ethanol was evaporated and the acidic mixture was poured into an extracting funnel containing 75 mL of ethyl acetate and 50 mL of HCl 1M and separated. The aqueous layer was washed with ethyl acetate. The aqueous phase was basified with pellets of NaOH and poured into an extracting funnel. The organic layer was washed with NaOH 1M and brine, dried over sodium sulfate, filtered, evaporated and dried under vacuum to give 544 mg (92%) of a yellow solid (Rf=0, 100% EtOAc, indicator: ninhydrin).

後処理

  1. customThe ethanol was evaporated
  2. additionthe acidic mixture was poured into an extracting funnel
  3. additioncontaining 75 mL of ethyl acetate and 50 mL of HCl 1M
  4. customseparated
  5. washThe aqueous layer was washed with ethyl acetate
  6. additionpoured into an extracting funnel
  7. washThe organic layer was washed with NaOH 1M and brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. customevaporated
  11. customdried under vacuum

出典と根拠

ORDレコード
ord-6dc7a7e18a4d44c69efd60d62a41adad
出典データセット
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06632816B1

反応ノート

読み込み中…

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