1,5-Naphthalenedisulfonic acid → HCID 131714450, 화합물

HRID 637667노트

반응식

HRID 637667 반응식
[CH3:1][CH2:2][C@@:3]1([OH:63])[CH2:21][N:19]2[CH2:20][CH:5]([CH2:6][C@:7]([C:59]([O:61][CH3:62])=[O:60])([C:22]3[CH:23]=[C:24]4[C@:32]56[C@@H:36]7[C@:37]([CH2:56][CH3:57])([C@@H:41]([O:52][C:53]([CH3:55])=[O:54])[C@@:42]8([O:48][C:46](=[O:47])[N:45]([CH2:49][CH2:50][Cl:51])[C:43]8=[O:44])[C@@H:31]5[N:30]([CH3:58])[C:25]4=[CH:26][C:27]=3[O:28][CH3:29])[CH:38]=[CH:39][CH2:40][N:35]7[CH2:34][CH2:33]6)[C:8]3[NH:16][C:15]4[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=4[C:9]=3[CH2:17][CH2:18]2)[CH2:4]1.[C:64]1([S:78]([OH:81])(=[O:80])=[O:79])[C:73]2[CH:72]=[CH:71][CH:70]=[C:69]([S:74]([OH:77])(=[O:76])=[O:75])[C:68]=2[CH:67]=[CH:66][CH:65]=1>CO>[CH3:1][CH2:2][C@@:3]1([OH:63])[CH2:21][N:19]2[CH2:20][CH:5]([CH2:6][C@:7]([C:59]([O:61][CH3:62])=[O:60])([C:22]3[CH:23]=[C:24]4[C@:32]56[C@@H:36]7[C@:37]([CH2:56][CH3:57])([C@@H:41]([O:52][C:53]([CH3:55])=[O:54])[C@@:42]8([O:48][C:46](=[O:47])[N:45]([CH2:49][CH2:50][Cl:51])[C:43]8=[O:44])[C@@H:31]5[N:30]([CH3:58])[C:25]4=[CH:26][C:27]=3[O:28][CH3:29])[CH:38]=[CH:39][CH2:40][N:35]7[CH2:34][CH2:33]6)[C:8]3[NH:16][C:15]4[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=4[C:9]=3[CH2:17][CH2:18]2)[CH2:4]1.[C:64]1([S:78]([O-:81])(=[O:80])=[O:79])[C:73]2[CH:72]=[CH:71][CH:70]=[C:69]([S:74]([O-:77])(=[O:76])=[O:75])[C:68]=2[CH:67]=[CH:66][CH:65]=1

참가 물질

4

반응물 2

HCID 66661,5-Naphthalenedisulfonic acidHCID 49967methyl (13S,17S)-13-[(1'R,5S,9'R,11'R,12'R,19'R)-11'-acetyloxy-3-(2-chloroethyl)-12'-ethyl-5'-methoxy-8'-methyl-2,4-dioxospiro[1,3-oxazolidine-5,10'-8,16-diazapentacyclo[10.6.1.01,9.02,7.016,19]nonadeca-2,4,6,13-tetraene]-4'-yl]-17-ethyl-17-hydroxy-1,11-diazatetracyclo[13.3.1.04,12.05,10]nonadeca-4(12),5,7,9-tetraene-13-carboxylate

생성물 1

HCID 131714450HCID 131714450, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To 1% (w/v) solution of vinzolidine free base (95+% purity) in methanol is added dropwise with stirring a stoichiometric amount (1 mole per mole) of a 2% methanolic solution of 1,5-naphthalenedisulfonic acid. The resulting solution was allowed to stand at ambient temperature for about two hours, during which time period crystallization of the vinzolidine 1,5-naphthalenedisulfonate salt begins. The crystallizing solution is kept at about 0° C. overnight and is then filtered. The filter cake is washed with a small amount of methanol and then dried in vacuo overnight at ambient temperature. The salt is then allowed to stand in air for about two hours. The yield of vinzolidine 1,5-naphthalenedisulfonate is 95-97%.

후처리

  1. customto stand at ambient temperature for about two hours, during which time period crystallization of the vinzolidine 1,5-naphthalenedisulfonate salt
  2. filtrationis then filtered
  3. washThe filter cake is washed with a small amount of methanol
  4. customdried in vacuo overnight at ambient temperature
  5. waitto stand in air for about two hours

출처 및 근거

ORD 기록
ord-efe1a20ce64e4286a46355cc154f3425
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558053

반응 노트

불러오는 중…