2,2'-Dipyridyl disulfide → HCID 178443924、化合物

HRID 24972

反応式

HRID 24972 の反応式
[CH3:1][CH:2]([CH2:4][CH2:5][CH2:6][C@H:7]([C@@H:9]1[C@:27]2([CH3:28])[C@H:12]([C@H:13]3[C@H:24]([CH2:25][CH2:26]2)[C@:22]2([CH3:23])[C:16]([CH2:17][C@H:18]([CH2:20][CH2:21]2)[OH:19])=[CH:15][CH2:14]3)[CH2:11][CH2:10]1)[CH3:8])[CH3:3].[CH2:29]([NH2:32])[CH2:30]N.C1[CH:38]=[C:37]([S:39][S:40]C2N=CC=CC=2)N=CC=1.[CH:47]([N:50](C(C)C)CC)(C)[CH3:48].[NH:56]=C1CCCS1.CC(CCC[C@H]([C@@H]1[C@]2(C)[C@H]([C@H]3[C@H](CC2)[C@]2(C)C(C[C@H](CC2)O)=CC3)CC1)C)C.C(N)CN.C1C=C(SSC2N=CC=CC=2)N=CC=1>C(Cl)Cl.CO>[CH3:3][CH:2]([CH2:4][CH2:5][CH2:6][C@H:7]([C@@H:9]1[C@:27]2([CH3:28])[C@H:12]([C@H:13]3[C@H:24]([CH2:25][CH2:26]2)[C@:22]2([CH3:23])[C:16]([CH2:17][C@H:18]([CH2:20][CH2:21]2)[OH:19])=[CH:15][CH2:14]3)[CH2:11][CH2:10]1)[CH3:8])[CH3:1].[CH2:47]([NH:50][C:29]([CH2:30][CH2:38][CH2:37][S:39][S:40][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][N:56]=1)=[NH:32])[CH3:48]

参加物

8

反応物 5

HCID 650932,2'-Dipyridyl disulfideHCID 81531DiisopropylethylamineHCID 4339412-IminothiolaneHCID 69752158Cholesterol Ethylenediamine2 回HCID 131723204Cholesterol ethylenediamine 2,2'-dipyridyldisulfide

生成物 1

HCID 178443924HCID 178443924、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

Pure cholesterol-ethylenediamine (10 mmol) was dissolved in 300 mL of DCM. 100 mmol of 2,2′-dipyridyl disulfide was dissolved in 100 mL of methanol and added to the cholesterol-ethylenediamine solution plus 20 mmol of diisopropylethylamine. 15 mmol of 2-iminothiolane was dissolved in 50 mL of methanol and then drop-wise added to the cholesterol-ethylenediamine/2,2′-dipyridyldisulfide solution over 30 minutes at R.T. Following an overnight R.T. stir, organic solvent was roto-evaporated away using medium vacuum until a minimal sample volume remained. Approximately 800 mL of acetonitrile was added to precipitate the crude product. The solid was then collected by filtration onto a Whatman #5 filter apparatus, rinsed several times with acetonitrile and then air-dried. The crude solid was dissolved in a minimal volume of chloroform and chromatographically purified using a silica column. The purified product presented a single TLC spot (4:1 chloroform/methanol), and a single peak (parent ion M+H=685) was identified by positive mode electrospray.

後処理

  1. customorganic solvent was roto-evaporated away
  2. additionApproximately 800 mL of acetonitrile was added
  3. customto precipitate the crude product
  4. filtrationThe solid was then collected by filtration onto a Whatman #5
  5. filtrationfilter apparatus
  6. washrinsed several times with acetonitrile
  7. customair-dried
  8. dissolutionThe crude solid was dissolved in a minimal volume of chloroform
  9. customchromatographically purified

出典と根拠

ORDレコード
ord-8f7ab44c45384625abf6313842637ab3
出典データセット
uspto-grants-2005_02
特許番号
US06858226B2

関連ノート

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