Dichloromethane → HCID 86757643、化合物

HRID 2268400ノート

反応式

HRID 2268400 の反応式
[OH:1][C@@H:2]([C@H:6]([OH:10])[C:7]([OH:9])=[O:8])[C:3]([OH:5])=[O:4].[C:11]1([CH:17]([C:50]2[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=2)[CH2:18][NH:19][C:20]2[N:28]=[C:27]([CH2:29][NH:30][CH:31]3[CH2:36][CH2:35][N:34]([CH:37]([CH3:39])[CH3:38])[CH2:33][CH2:32]3)[N:26]=[C:25]3[C:21]=2[N:22]=[CH:23][N:24]3[C@H:40]2[C@H:44]([OH:45])[C@H:43]([OH:46])[C@@H:42]([CH2:47][O:48][CH3:49])[O:41]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.ClCCl>C(O)(C)C>[OH:1][C@@H:2]([C@H:6]([OH:10])[C:7]([OH:9])=[O:8])[C:3]([OH:5])=[O:4].[C:11]1([CH:17]([C:50]2[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=2)[CH2:18][NH:19][C:20]2[N:28]=[C:27]([CH2:29][NH:30][CH:31]3[CH2:36][CH2:35][N:34]([CH:37]([CH3:38])[CH3:39])[CH2:33][CH2:32]3)[N:26]=[C:25]3[C:21]=2[N:22]=[CH:23][N:24]3[C@H:40]2[C@H:44]([OH:45])[C@H:43]([OH:46])[C@@H:42]([CH2:47][O:48][CH3:49])[O:41]2)[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 439655D-Tartaric acidHCID 9895232HCID 9895232、化合物

生成物 1

HCID 86757643HCID 86757643、化合物収率 15.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒4 回

実験手順

A solution of (2S,3S)-2,3-dihydroxybutanedioic acid (49 mg, 0.33 mmol) in isopropyl alcohol (1 ml) was added to a stirred solution of [((2R,3R,4S,5R)-2-(6-[(2,2-diphenylethyl)amino]-2-{[(1-isopropyl-4-piperidinyl)amino]methyl}-9H-purin-9-yl)-5-(methoxymethyl)tetrahydro-3,4-furandiol (200 mg, 0.33 mmol) (example 16) in isopropyl alcohol (1 ml). This resulted in the formation of a thick precipitate, which was dissolved by the addition of dichloromethane and isopropyl alcohol. The solvent was boiled off from the solution until a gum started to appear and then more isopropyl alcohol was added. The resulting white crystalline solid was filtered off, dried and then recrystallized from hot ethanol to give the title compound (40 mg) as a white powder. M.p. 161-163° C.

後処理

  1. customThis resulted in the formation of a thick precipitate, which
  2. filtrationThe resulting white crystalline solid was filtered off
  3. customdried
  4. customrecrystallized from hot ethanol

出典と根拠

ORDレコード
ord-a4b353ba813e4c70907cc1587aaacb3f
出典データセット
uspto-grants-2001_12
特許番号
US06326359B1

反応ノート

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