Dichloromethane → HCID 86757643, 화합물

HRID 2268400노트

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HRID 2268400 반응식
[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

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 439655D-Tartaric acidHCID 9895232HCID 9895232, 화합물

생성물 1

HCID 86757643HCID 86757643, 화합물수율 15.8%

시약·촉매·용매 1

HCID 3776Isopropanol용매4회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a4b353ba813e4c70907cc1587aaacb3f
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06326359B1

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