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4-Methylmorpholine → HCID 67114148、化合物

HRID 2245226
ノート
印刷プレビュー

反応式

HRID 2245226 の反応式
[CH:1]1([CH:7]([NH:30][C:31]([C:33]2[CH:38]=[N:37][CH:36]=[CH:35][N:34]=2)=[O:32])[C:8]([NH:10][CH:11]([C:26]([CH3:29])([CH3:28])[CH3:27])[C:12]([N:14]2[CH:22]3[CH:17]([CH2:18][CH2:19][CH2:20][CH2:21]3)[CH2:16][CH:15]2[C:23](O)=[O:24])=[O:13])=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.CN1CCOCC1.Cl.[CH2:80]([O:82][C:83](=[O:91])[CH:84]([OH:90])[CH:85]([NH2:89])[CH2:86][CH2:87][CH3:88])[CH3:81]>O.ClCCl.CN(C)C=O>[CH2:80]([O:82][C:83](=[O:91])[CH:84]([OH:90])[CH:85]([NH:89][C:23]([CH:15]1[CH2:16][CH:17]2[CH:22]([CH2:21][CH2:20][CH2:19][CH2:18]2)[N:14]1[C:12](=[O:13])[CH:11]([NH:10][C:8](=[O:9])[CH:7]([CH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[NH:30][C:31]([C:33]1[CH:38]=[N:37][CH:36]=[CH:35][N:34]=1)=[O:32])[C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:86][CH2:87][CH3:88])[CH3:81]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-Methylmorpholine2 回HCID 2724699PyBOPHCID 684917401-(2-{2-Cyclohexyl-2-[(pyrazine-2-carbonyl)-amino]-acetylamino}-3,3-dimethyl-butyryl)-octahydro-indole-2-carboxylic acidHCID 85806087Ethyl 3-amino-2-hydroxyhexanoate hydrochloride

生成物 1

HCID 67114148HCID 67114148、化合物収率 82%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 22350042dichloromethane N,N-dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

In a dry flask charged with a 1:1 mixture of dichloromethane-dimethylformamide (100 ml) was placed 1-(2-{2-Cyclohexyl-2-[(pyrazine-2-carbonyl)-amino]-acetylamino}-3,3-dimethyl-butyryl)-octahydro-indole-2-carboxylic acid 32a (2.0 g, 4.28 mmols), PyBOP (2.5 g, 4.7 mmol), and N-methyl-morpholine (2.4 ml, 21.4 mmol) and the reaction placed under an atmosphere of nitrogen. In a 100 mL addition funnel was placed a solution of the amine 14 (1.0 g, 4.7 mmols) and N-methyl-morpholine (0.60 ml, 5.35 mmol) in a 1:1 mixture of dichloromethane-dimethylformamide (10 ml). The reaction was cooled to 0° C., and the amine was added while maintaining the temperature at 0° C. The reaction was allowed to warm to ambient temperature as it was stirred over night. HPLC analysis showed the reaction to be complete, and then the reaction was diluted with water to 500 mL. After stirring the precipitate was filtered and dried to give 2.4 g (82% yield) of 32 as a beige solid. This material was used as is in the next step without further purification. HPLC: RT=5.66 min, (10-90% acetonitrile-water over 7 minutes); LC/MS: retention time 3.94 min (10-90% acetonitrile-water over 5 minutes); M+H+=685.5.

後処理

  1. additionIn a 100 mL addition funnel
  2. temperaturewhile maintaining the temperature at 0° C
  3. temperatureto warm to ambient temperature as it
  4. customthe reaction
  5. stirringAfter stirring the precipitate
  6. filtrationwas filtered
  7. customdried

出典と根拠

ORDレコード
ord-2fd893c7f63f40a9a17f4e50be69d23a
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07683033B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート