Water → HCID 86602730, 화합물

HRID 1244821노트

반응식

HRID 1244821 반응식
Cl.[Cl:2][CH2:3][CH2:4][CH2:5][C:6]#[C:7][C:8]([NH2:11])([CH3:10])[CH3:9].C(N(CC)CC)C.[Br:19][CH:20]([CH2:24][CH3:25])[C:21](Br)=[O:22].O>ClCCl>[Br:19][CH:20]([CH2:24][CH3:25])[C:21]([NH:11][C:8]([CH3:10])([CH3:9])[C:7]#[C:6][CH2:5][CH2:4][CH2:3][Cl:2])=[O:22]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 1172932-Bromobutanoyl bromideHCID 86602731HCID 86602731, 화합물

생성물 1

HCID 86602730HCID 86602730, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
5 °C

실험 절차

The product from Step 2 (12.2 g) was suspended in dry dichloromethane (300 ml), cooled to 5° C. with stirring and dry triethylamine (18.1 ml) was added. The mixture was stirred for 0.25 hours and 2-bromobutyryl bromide (14.3 g) in dichloromethane (25 ml) was added dropwise over 0.5 hours at 10–18° C. The mixture was stirred for a further 0.5 hours then allowed to warm to ambient temperature for 2 hours and stored for 18 hours. Water was added and the organic phase was separated, washed with water (three times), dried over magnesium sulphate then evaporated under reduced pressure to give the required product as a dark yellow oil, 17.4 g, 1H NMR (CDCl3) δ: 1.04(3H, t); 1.62(6H, s); 1.96(2H, m); 2.10(2H, m); 2.38(2H, m); 3.66(2H, t); 4.12(1H, t); 6.44(1H, s).

후처리

  1. stirringThe mixture was stirred for 0.25 hours
  2. stirringThe mixture was stirred for a further 0.5 hours
  3. temperatureto warm to ambient temperature for 2 hours
  4. customthe organic phase was separated
  5. washwashed with water (three times)
  6. dry with materialdried over magnesium sulphate
  7. customthen evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-010885194af44b95979420a08d126978
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122672B2

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