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1,2-Dichloroethane → 1-(2-{2-[(3-acetyl-4,5-dimethyl-1H-pyrrole-2-carbonyl)-amino]-2-cyclohexyl-acetylamino}-3,3-dimethyl-butyryl)-octahydro-indole-2-carboxylic acid tert-butyl ester

HRID 917800
ノート
印刷プレビュー

反応式

HRID 917800 の反応式
[C:1]([C:4]1[C:8]([CH3:9])=[C:7]([CH3:10])[NH:6][C:5]=1[C:11]([OH:13])=O)(=[O:3])[CH3:2].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[C:28]([O:32][C:33]([CH:35]1[CH2:43][CH:42]2[CH:37]([CH2:38][CH2:39][CH2:40][CH2:41]2)[N:36]1[C:44](=[O:61])[CH:45]([NH:50][C:51](=[O:60])[CH:52]([NH2:59])[CH:53]1[CH2:58][CH2:57][CH2:56][CH2:55][CH2:54]1)[C:46]([CH3:49])([CH3:48])[CH3:47])=[O:34])([CH3:31])([CH3:30])[CH3:29]>CN(C=O)C>[C:28]([O:32][C:33]([CH:35]1[CH2:43][CH:42]2[CH:37]([CH2:38][CH2:39][CH2:40][CH2:41]2)[N:36]1[C:44](=[O:61])[CH:45]([NH:50][C:51](=[O:60])[CH:52]([NH:59][C:11]([C:5]1[NH:6][C:7]([CH3:10])=[C:8]([CH3:9])[C:4]=1[C:1](=[O:3])[CH3:2])=[O:13])[CH:53]1[CH2:54][CH2:55][CH2:56][CH2:57][CH2:58]1)[C:46]([CH3:49])([CH3:48])[CH3:47])=[O:34])([CH3:29])([CH3:30])[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 5906793-Acetyl-4,5-dimethyl-1H-pyrrole-2-carboxylic acidHCID 684969241-[2-(2-Amino-2-cyclohexyl-acetylamino)-3,3-dimethyl-butyryl]-octahydro-indole-2-carboxylic acid tert-butyl ester

生成物 1

HCID 68492991
1-(2-{2-[(3-acetyl-4,5-dimethyl-1H-pyrrole-2-carbonyl)-amino]-2-cyclohexyl-acetylamino}-3,3-dimethyl-butyryl)-octahydro-indole-2-carboxylic acid tert-butyl ester
収率 85%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

3-acetyl-4,5-dimethyl-2-pyrrole carboxylic acid 10b (2.5 g, 13.7 mmol) in DMF (56 mL) was treated with EDC (2.75 g, 14.4 mmol) and HOBt (2.20 g, 14.4 mmol) and stirred at RT for 15 minutes. Amine 16b (6.23 g, 13.0 mmol) in DMF (10 mL) was added, the reaction mixture stirred at RT and monitored by HPLC. The mixture was concentrated in vacuo, then dissolved in EtOAc. 1.0N glycine sodium salt aqueous solution was added until all excess amino ester 16b was consumed (several hours). The mixture was washed with 1N HCl (3×), brine, bicarb (3×), and brine, then dried over sodium sulfate, filtered, and concentrated in vacuo. Purification through a short plug of silica gel (25%EA/Hex) afforded 7.08 g, (85%) of 1-(2-{2-[(3-acetyl-4,5-dimethyl-1H-pyrrole-2-carbonyl)-amino]-2-cyclohexyl-acetylamino}-3,3-dimethyl-butyryl)-octahydro-indole-2-carboxylic acid tert-butyl ester 17b.

後処理

  1. stirringthe reaction mixture stirred at RT
  2. concentrationThe mixture was concentrated in vacuo
  3. dissolutiondissolved in EtOAc
  4. addition1.0N glycine sodium salt aqueous solution was added until all excess amino ester 16b
  5. customwas consumed (several hours)
  6. washThe mixture was washed with 1N HCl (3×), brine, bicarb (3×), and brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customPurification through a short plug of silica gel (25%EA/Hex)

出典と根拠

ORDレコード
ord-f3ff062e77a84ee7b330cbca0ab881eb
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07273885B2

反応ノート

読み込み中…

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