Tetrahydrofuran → HCID 462612, 화합물

HRID 743092노트

반응식

HRID 743092 반응식
C(N(CC)CC)C.[CH:8]1([C:11](Cl)=[O:12])[CH2:10][CH2:9]1.[OH:14][CH2:15][C:16]1[S:17][S:18][C:19]([CH2:22][OH:23])=[CH:20][CH:21]=1.S1C=CC=CS1.[O:30]1[CH2:34][CH2:33][CH2:32][CH2:31]1>CCOCC>[CH:8]1([C:11]([O:14][CH2:15][C:16]2[S:17][S:18][C:19]([CH2:22][O:23][C:34]([CH:33]3[CH2:31][CH2:32]3)=[O:30])=[CH:20][CH:21]=2)=[O:12])[CH2:10][CH2:9]1

참가 물질

7

반응물 5

HCID 8028Tetrahydrofuran2회HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 462608[6-(Hydroxymethyl)dithiin-3-yl]methanolHCID 120445651,2-Dithiin

생성물 1

HCID 462612HCID 462612, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a stirred solution of triethylamine (0.30 mL) in tetrahydrofuran (2.0 mL) at 0° C. was added dropwise cyclopropanecarbonyl chloride (0.10 mL) followed by the addition of 3,6-bis(hydroxymethyl)-1,2-dithiin, Dithiin A (20 mg, 0.113 mmol) in tetrahydrofuran (1.0 mL). After stirring in the dark at room temperature overnight the mixture was diluted with ether (20 mL) and partitioned between 1.0M H3PO4 (80 mL) and diethyl ether (30 mL). The diethyl ether layer was washed with saturated NaHCO3 (100 mL), dried (Na2SO4), and evaporated to give a red oil (31.5 mg): 1H NMR (CDCl3) δ6.38 (s, 2H), 4.71 (s, 4H), 1.67 (m, 2H), 1.04 (m, 4H), 0.92 (m, 4H).

후처리

  1. custompartitioned between 1.0M H3PO4 (80 mL) and diethyl ether (30 mL)
  2. washThe diethyl ether layer was washed with saturated NaHCO3 (100 mL)
  3. dry with materialdried (Na2SO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-29a21e21d3714fc7849276b899627a55
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556875

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