Pyridine → Borate(1-), tetrafluoro-, hydrogen, compd. with pyridine (1:1:1)

HRID 979182

반응식

HRID 979182 반응식
CNCC(OC)OC.[N:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[F:15][B-:16]([F:19])([F:18])[F:17].N#[O+]>C1COCC1>[F:15][B-:16]([F:19])([F:18])[F:17].[NH+:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 85032,2-DimethoxyethylmethylamineHCID 11137142Nitrilooxonium tetrafluoroborate

생성물 1

HCID 11019233Borate(1-), tetrafluoro-, hydrogen, compd. with pyridine (1:1:1)

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 1-(methylamino)-2,2-dimethoxyethane (132.6 g; 1.11 mol) and pyridine (94.5 ml; 1.17 mol) in THF (1.3 ) was brought to 0°-5° C. with an ice-bath and nitrosonium tetrafluoroborate (139.5 g; 1.19 mol) was added in portions over 35 minutes. Fuming was observed and the temperature of the reaction mixture was kept below 20° C. throughout the addition. After stirring an additional 20 minutes, the white solid which had formed (pyridinium tetrafluoroborate) was filtered and CH2Cl2 and H2O were added. The organic phase was washed a second time with H2O, dried (anhyd. Na2CO3) and concentrated in vacuo at 40° C. to yield an amber oil. This oil was distilled at vacuum pump pressure (2-4 mm Hg) to yield Compound (XXVII-A), N-Methyl-N-(2,2-dimethoxyethyl)nitrosoamine (73.0 g; 44%) as a yellow liquid: bp 75°-85° C. Both TLC and NMR indicated a mixture of Z and E isomers.

후처리

  1. additionthe temperature of the reaction mixture was kept below 20° C. throughout the addition

출처 및 근거

ORD 기록
ord-bc1e8cbda56e43519ace621edf809d42
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666906

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