Water → 1,1-Dimethylethyl N-[3-methyl-1-(phenylmethyl)-3-pyrrolidinyl]carbamate

HRID 69498ノート

反応式

HRID 69498 の反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][C:10]([CH3:16])(C(O)=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([N:19]([CH2:22]C)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:31])C=CC=CC=1.O.[C:42]([OH:46])([CH3:45])([CH3:44])[CH3:43]>>[C:42]([O:46][C:22](=[O:31])[NH:19][C:10]1([CH3:16])[CH2:11][CH2:12][N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH2:9]1)([CH3:45])([CH3:44])[CH3:43]

参加物

6

反応物 5

HCID 962WaterHCID 6386tert-ButanolHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 36840571-Benzyl-3-methylpyrrolidine-3-carboxylic acid

生成物 1

HCID 104937341,1-Dimethylethyl N-[3-methyl-1-(phenylmethyl)-3-pyrrolidinyl]carbamate

実験手順

A solution of 1-benzyl-3-methyl-pyrrolidine-3-carboxylic acid (500 mg), triethylamine (231 mg) and diphenylphosphoryl azide (640 mg) in tert-butanol (15 mL) was stirred at 95° C. for 4 h. After adding water it was extracted with dichloromethane, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel. In this way the product was obtained with molecular weight 290.41 (C17H26N2O2); MS (ESI): 291 (M+H+).

後処理

  1. extractionwas extracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was chromatographed on silica gel
  5. customIn this way the product was obtained with molecular weight 290.41 (C17H26N2O2)

出典と根拠

ORDレコード
ord-b7b576ecc6d64312ac4a75c1fbd3111d
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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