Sodium Bisulfate → HCID 14473226, 화합물

HRID 2106900

반응식

HRID 2106900 반응식
[CH3:1][O:2][C:3]1[C:7]([CH2:8][CH2:9][CH2:10][CH3:11])=[CH:6][S:5][CH:4]=1.Br[C:13]1[C:17]([CH2:18][CH2:19]CC)=CS[CH:14]=1.C[O-].[Na+].OS([O-])(=O)=O.[Na+]>CO.C(O)CCCCC.C1(C)C=CC=CC=1>[CH2:1]([O:2][C:3]1[C:7]([CH2:8][CH2:9][CH2:10][CH3:11])=[CH:6][S:5][CH:4]=1)[CH2:14][CH2:13][CH2:17][CH2:18][CH3:19]

참가 물질

8

반응물 4

HCID 516919Sodium BisulfateHCID 10942334Sodium MethoxideHCID 125026793-Bromo-4-butylthiopheneHCID 19099073HCID 19099073, 화합물

생성물 1

HCID 14473226HCID 14473226, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 1140Toluene용매HCID 81031-Hexanol용매

실험 절차

10 g of 3-methoxy-4-butylthiophene, prepared from 3-bromo-4-butylthiophene by reaction with sodium methylate in methanol with catalysis by CuO, b.p. 54° C./0.26 mbar, were dissolved as in Example 14 in 50 cm3 of 1-hexanol and 30 ml of toluene, and 1 g of NaHSO4 was added. After distilling off 6 cm3 of azeotrope, the batch was worked up as in Example 14. Yield 8.5 g of 3-hexyloxy-4-butylthiophene of b.p. 112° to 116° C./0.26 mbar, which corresponds to 60% of theory.

후처리

  1. distillationAfter distilling off 6 cm3 of azeotrope

출처 및 근거

ORD 기록
ord-fae56391e3174a5ba90dc7325230c000
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04931568

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