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Trifluoroacetic acid → HCID 178504906、化合物

HRID 1257725
ノート
印刷プレビュー

反応式

HRID 1257725 の反応式
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([S:14]([CH3:17])(=[O:16])=[O:15])[CH2:10][CH2:9]1)(C)(C)C.[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22]>C(Cl)Cl>[F:19][C:20]([F:25])([F:24])[C:21]([OH:23])=[O:22].[CH3:17][S:14]([C@H:11]1[CH2:12][CH2:13][C@H:8]([NH2:7])[CH2:9][CH2:10]1)(=[O:15])=[O:16]
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 6422Trifluoroacetic acidHCID 178454083HCID 178454083、化合物

生成物 1

HCID 178504906HCID 178504906、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A suspension of trans (4-methanesulfonyl-cyclohexyl)-carbamic acid tert-butyl ester (0.40 g, 1.40 mmol) in DCM (5 mL) was treated with trifluoroacetic acid (5 mL) and the mixture was stirred at ambient temperature for 30 minutes then concentrated under vacuum. The residue was azeotroped with toluene (×2) and the resulting oil was triturated (diethyl ether) to provide a solid which was washed with ether and dried to give 386 mg (93%) of trans 4-methanesulfonyl-cyclohexylamine trifluoroacetic acid salt as a white solid. 1H NMR (400 MHz, DMSO) δ: 7.86 (s, 3H), 3.11-2.98 (m, 2H), 2.92 (s, 3H), 2.18-2.02 (m, 4H), 1.56-1.43 (m, 2H), 1.43-1.28 (t, 2H).

後処理

  1. concentrationthen concentrated under vacuum
  2. customThe residue was azeotroped with toluene (×2)
  3. customthe resulting oil was triturated (diethyl ether)
  4. customto provide a solid which
  5. washwas washed with ether
  6. customdried

出典と根拠

ORDレコード
ord-7d17196c44964e14bc31803dfaff1eec
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461328B2

反応ノート

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