Diisopropylethylamine → HCID 25206131、化合物

HRID 387639ノート

反応式

HRID 387639 の反応式
Cl.[NH2:2][C@@H:3]([CH2:21][C:22]1[CH:27]=[C:26]([F:28])[CH:25]=[C:24]([F:29])[CH:23]=1)[C@H:4]([OH:20])[CH2:5][NH:6][C:7]1([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)[CH2:9][CH2:8]1.[O:30]=[C:31]1[C:40]2[CH:39]=[CH:38][CH:37]=[C:36]([C:41](O)=[O:42])[C:35]=2[CH2:34][CH2:33][N:32]1[CH2:44][CH2:45][CH2:46][CH2:47][CH3:48].OC1C2N=NNC=2C=CC=1.Cl.CN(C)CCCN=C=NCC.C(N(CC)C(C)C)(C)C>ClCCl.C(OCC)C.O>[F:29][C:24]1[CH:23]=[C:22]([CH:27]=[C:26]([F:28])[CH:25]=1)[CH2:21][C@H:3]([NH:2][C:41]([C:36]1[C:35]2[CH2:34][CH2:33][N:32]([CH2:44][CH2:45][CH2:46][CH2:47][CH3:48])[C:31](=[O:30])[C:40]=2[CH:39]=[CH:38][CH:37]=1)=[O:42])[C@H:4]([OH:20])[CH2:5][NH:6][C:7]1([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:17])([F:18])[F:19])[CH:11]=2)[CH2:9][CH2:8]1

参加物

9

反応物 5

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 68469137HCID 68469137、化合物HCID 86643873HCID 86643873、化合物HCID 178418300HCID 178418300、化合物

生成物 1

HCID 25206131HCID 25206131、化合物収率 81.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

326 mg of (2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)butan-2-ol hydrochloride (2:1), 180 mg of 1-oxo-2-pentyl-1,2,3,4-tetrahydroisoquinoline-5-carboxylic acid, 14 mg of hydroxybenzotriazole, 165 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 0.47 cm3 of N,N-diisopropylethylamine in 18 cm3 of dichloromethane are stirred for 20 h at a temperature close to 20° C. 10 cm3 of water and dichloromethane are added to the reaction medium. The suspension is filtered, washed successively with water and dichloromethane. The solid obtained is taken up in ethyl ether, filtered, washed with ethyl ether and dried under vacuum at 20° C. 360 mg of N-[(1S,2R)-1-(3,5-difluorobenzyl)-2-hydroxy-3-({1-[3-(trifluoromethyl)phenyl]cyclopropyl}amino)propyl]-1-oxo-2-pentyl-1,2,3,4-tetrahydroisoquinoline-5-carboxamide are obtained in the form of a white solid.

後処理

  1. customclose to 20° C
  2. filtrationThe suspension is filtered
  3. washwashed successively with water and dichloromethane
  4. customThe solid obtained
  5. filtrationfiltered
  6. washwashed with ethyl ether
  7. customdried under vacuum at 20° C

出典と根拠

ORDレコード
ord-5cf512d38e904e35a981dbc59998b077
出典データセット
uspto-grants-2013_02
特許番号
US08372864B2

反応ノート

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