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Water → (2s,3s)-5-{2-[(5-{[(Benzyloxy)carbonyl]amino}pentyl)amino]-2-oxoethyl}-2-[(3-phenylpyrrolidin-1-yl)carbonyl]piperidine-3-carboxylic acid

HRID 61431
ノート
印刷プレビュー

反応式

HRID 61431 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18](=[O:46])[CH2:19][CH:20]1[CH2:25][NH:24][C@H:23]([C:26]([N:28]2[CH2:32][CH2:31][CH:30]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[CH2:29]2)=[O:27])[C@@H:22]([C:39]([O:41]C(C)(C)C)=[O:40])[CH2:21]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.FC(F)(F)C(O)=O>C(Cl)Cl>[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18](=[O:46])[CH2:19][CH:20]1[CH2:25][NH:24][C@H:23]([C:26]([N:28]2[CH2:32][CH2:31][CH:30]([C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)[CH2:29]2)=[O:27])[C@@H:22]([C:39]([OH:41])=[O:40])[CH2:21]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 67304960Tert-butyl (2s,3s)-5-{2-[(5-{[(benzyloxy)carbonyl]amino}pentyl)amino]-2-oxoethyl}-2-[(3-phenylpyrrolidin-1-yl)carbonyl]piperidine-3-carboxylate

生成物 1

HCID 67304154(2s,3s)-5-{2-[(5-{[(Benzyloxy)carbonyl]amino}pentyl)amino]-2-oxoethyl}-2-[(3-phenylpyrrolidin-1-yl)carbonyl]piperidine-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

A solution of tert-butyl(2S,3S)-5-{2-[(5-{[(benzyloxy)carbonyl]amino}pentyl)amino]-2-oxoethyl}-2[(3-phenylpyrrolidin-1-yl)carbonyl]piperidine-3-carboxylate (40 mg, 0.063 mmol) in methylene chloride (2 mL) was added a drop of water and trifluoroacetic acid (4 mL). After stirring the reaction mixture overnight, the volatiles were removed in-vacuo and the residue was azeotropically washed with benzene (2×3 mL) and heptane (2×3 mL). The crude product was dried under high vacuum and used directly in the following coupling reaction without purification. MS (ESI): 579 (M+H).

後処理

  1. customthe volatiles were removed in-vacuo
  2. washthe residue was azeotropically washed with benzene (2×3 mL) and heptane (2×3 mL)
  3. dry with materialThe crude product was dried under high vacuum
  4. customused directly in the following coupling reaction without purification

出典と根拠

ORDレコード
ord-da6e3da6d34240bf8124b65a1654f4c6
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440958B2

反応ノート

読み込み中…

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