Triethylamine → HCID 86753273、化合物

HRID 355337

反応式

HRID 355337 の反応式
[CH:1]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[C:4](=[O:9])[O:3][C:2]2=[O:10].C(N(CC)CC)C.Cl.[CH2:19]([NH:26][O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(Cl)Cl>[C:29]1([CH2:28][O:27][N:26]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:4]([C@@H:5]2[CH2:6][CH2:7][C@H:1]([C:2]([OH:3])=[O:10])[CH2:8]2)=[O:9])[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2397991,3-Cyclopentanedicarboxylic anhydrideHCID 18358890N-(Benzyloxy)-1-phenylmethanamine--hydrogen chloride (1/1)

生成物 1

HCID 86753273HCID 86753273、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

552 mg of 3-Oxabicyclo[3.2.1]octane-2,4-dione (3.94 mmol, prepared according to the procedure described in Chem. Lett., p 93, (1994)) is added to a rapidly stirring solution of triethylamine (0.55 mL, 3.94 mmol) and N-benzyl-O-benzylhydroxylamine hydrochloride (983 mg, 3.94 mmol) in CH2Cl2 in a flame dried flask under nitrogen. After stirring at ambient temperature for 3 days, the reaction is quenched with aqueous citric acid (1M). Extraction into CH2Cl2 (3×50 mL), followed by drying over MgSO4, yielded a pale yellow oil, 1.51 g. Recrystallization in ethyl acetate/hexane provided the product as a white crystalline solid, 1.32 g (95%). mp. 118°-120° C.

後処理

  1. customdried flask under nitrogen
  2. customthe reaction is quenched with aqueous citric acid (1M)
  3. extractionExtraction into CH2Cl2 (3×50 mL)
  4. dry with materialby drying over MgSO4
  5. customyielded a pale yellow oil, 1.51 g
  6. customRecrystallization in ethyl acetate/hexane

出典と根拠

ORDレコード
ord-a9acd726059349c9be9f4de5bfaaf32b
出典データセット
uspto-grants-1998_11
特許番号
US05830869

関連ノート

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