p-Toluenesulfonic acid → HCID 86735829、化合物

HRID 866367ノート

反応式

HRID 866367 の反応式
[S:1]1[CH2:5][CH2:4][S:3][CH:2]1[CH2:6][CH2:7][CH:8]1[CH:19](/[CH:20]=[CH:21]/[CH:22]([OH:28])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:18][CH2:17][C:9]21[O:14][CH2:13][C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2.C1(C)C=CC(S(O)(=O)=O)=CC=1.[O:40]1[CH:45]=[CH:44][CH2:43][CH2:42][CH2:41]1.C([O-])([O-])=O.[Na+].[Na+]>CCOCC>[S:1]1[CH2:5][CH2:4][S:3][CH:2]1[CH2:6][CH2:7][CH:8]1[CH:19](/[CH:20]=[CH:21]/[CH:22]([OH:28])[CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[CH2:18][CH2:17][C:9]21[O:14][CH2:13][C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2.[O:40]1[CH2:41][CH2:42][CH2:43][CH2:44][CH:45]1[O:14][CH:9]1[CH2:17][CH2:18][CH2:19][CH2:20][O:10]1

参加物

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyran2 回HCID 10340Sodium CarbonateHCID 203869041-[7-[(1,3-Dithia-2-cyclopentyl)-ethyl]-3,3-dimethyl-1,5-dioxaspiro[5,4]-dec-8-yl]-trans-1-octene-3-ol

生成物 1

HCID 86735829HCID 86735829、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

1.1 g (2.5 mmoles of 1-[7-[(1,3-dithia-2-cyclopentyl)-ethyl]-3,3-dimethyl-1,5-dioxaspiro[5,4]-dec-8-yl]-trans-1-octene-3-ol were dissolved in 20 ml of absolute ether, 20 mg of p-toluenesulfonic acid were added, 1.2 ml (13 mmoles) of dihydropyrane in 10 ml of absolute ether were added dropwise and the whole was stirred for 4 hours at room temperature. 0.2 ml of dihydropyrane was again added. The reaction mixture was allowed to stand overnight and was then stirred for 30 minutes with 0.5 g of solid Na2CO3. The suspension was filtered, the filtrate was concentrated under reduced pressure and the oil that had formed was eluted with cyclohexane-ethyl acetate (9:1) over a silica gel column.

後処理

  1. waitto stand overnight
  2. filtrationThe suspension was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customthe oil that had formed
  5. washwas eluted with cyclohexane-ethyl acetate (9:1) over a silica gel column

出典と根拠

ORDレコード
ord-b5ed18aee1354a4a91a8ea2251114516
出典データセット
uspto-grants-1978_07
特許番号
US04098815

反応ノート

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