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Triethylamine → tert-butyl [(R)-2-(3-cyclopropylmethoxy-3-o-tolylazetidin-1-yl)-1-(4-methoxybenzyl)-2-oxoethyl]carbamate

HRID 530694
ノート
印刷プレビュー

反応式

HRID 530694 の反応式
Cl.C(N=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1.C(N(CC)CC)C.Cl.[CH:31]1([CH2:34][O:35][C:36]2([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=3[CH3:46])[CH2:39][NH:38][CH2:37]2)[CH2:33][CH2:32]1.[C:47]([O:51][C:52]([NH:54][C@H:55]([CH2:59][C:60]1[CH:65]=[CH:64][C:63]([O:66][CH3:67])=[CH:62][CH:61]=1)[C:56](O)=[O:57])=[O:53])([CH3:50])([CH3:49])[CH3:48]>CN(C)C=O.CCCCCCC.C(OCC)(=O)C>[CH:31]1([CH2:34][O:35][C:36]2([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=3[CH3:46])[CH2:37][N:38]([C:56](=[O:57])[C@H:55]([NH:54][C:52](=[O:53])[O:51][C:47]([CH3:48])([CH3:49])[CH3:50])[CH2:59][C:60]3[CH:61]=[CH:62][C:63]([O:66][CH3:67])=[CH:64][CH:65]=3)[CH2:39]2)[CH2:32][CH2:33]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 7017908Boc-O-methyl-D-tyrosineHCID 711523703-Cyclopropylmethoxy-3-o-tolylazetidine hydrochloride

生成物 1

HCID 86729200
tert-butyl [(R)-2-(3-cyclopropylmethoxy-3-o-tolylazetidin-1-yl)-1-(4-methoxybenzyl)-2-oxoethyl]carbamate
収率 41.8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 21899848Ethylacetate heptane溶媒

実験手順

1.9 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (10.2 mmol), 1.4 g of N-hydroxybenzotriazole (10.2 mmol), 3.8 ml of triethylamine (27.2 mmol) and then 2.2 g (8.7 mmol) of 3-cyclopropylmethoxy-3-o-tolylazetidine hydrochloride dissolved in 35 ml of N,N-dimethylformamide are successively added to a solution of 2.7 g (9.2 mmol) of (R)-2-tert-butoxycarbonylamino-3-(4-methoxyphenyl)propanoic acid in 55 ml of N,N-dimethylformamide. The reaction medium is stirred at room temperature for 38 hours. A 1/1 heptane/ethyl acetate mixture is added and the reaction medium is washed with aqueous 1N sodium hydroxide solution. The organic phase is then washed with aqueous 1N hydrochloric acid solution, dried over sodium sulfate, filtered and concentrated under vacuum. 2.7 g of crude residue are obtained and are purified by chromatography on silica gel eluted with a heptane/ethyl acetate mixture, the polarity being increased from 95/5 to 60/40. 1.8 g (41%) of tert-butyl [(R)-2-(3-cyclopropylmethoxy-3-o-tolylazetidin-1-yl)-1-(4-methoxybenzyl)-2-oxoethyl]carbamate are obtained in the form of a white solid.

後処理

  1. washthe reaction medium is washed with aqueous 1N sodium hydroxide solution
  2. washThe organic phase is then washed with aqueous 1N hydrochloric acid solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. custom2.7 g of crude residue are obtained
  7. customare purified by chromatography on silica gel
  8. washeluted with a heptane/ethyl acetate mixture
  9. temperaturethe polarity being increased from 95/5 to 60/40

出典と根拠

ORDレコード
ord-42e3484d30c846f7a9a2b5360cf1dca4
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353083B2

反応ノート

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