p-Toluenesulfonic acid → HCID 86735829, 화합물

HRID 866367노트

반응식

HRID 866367 반응식
[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

참가 물질

6

반응물 4

HCID 6101p-Toluenesulfonic acidHCID 80803,4-dihydro-2H-pyran2회HCID 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

생성물 1

HCID 86735829HCID 86735829, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b5ed18aee1354a4a91a8ea2251114516
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04098815

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