Hydrochloric Acid → N-(11-Amino-2,2,12-trimethyltrideca-4,8-dien-1-ylidene)hydroxylamine

HRID 128042

반응식

HRID 128042 반응식
[CH3:1][C:2]1([CH3:17])[CH2:13][CH:12]=[CH:11][CH2:10][CH2:9][CH:8]=[CH:7][CH2:6][CH:5]([CH:14]([CH3:16])[CH3:15])[N:4]=[CH:3]1.Cl.Cl.[NH2:20][OH:21].[OH-].[Na+]>O>[CH3:1][C:2]([CH3:17])([CH2:13][CH:12]=[CH:11][CH2:10][CH2:9][CH:8]=[CH:7][CH2:6][CH:5]([CH:14]([CH3:16])[CH3:15])[NH2:4])[CH:3]=[N:20][OH:21]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 5575123,3-Dimethyl-12-isopropyl-1-aza-1,5,9-cyclododecatriene

생성물 1

HCID 71403854N-(11-Amino-2,2,12-trimethyltrideca-4,8-dien-1-ylidene)hydroxylamine수율 92%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

233.4 g (1 mol) of 3,3-dimethyl-12-isopropyl-1-aza-1,5,9-cyclododecatriene is added dropwise to 100 g of 37% hydrochloric acid and 200 ml of water in the course of one hour, in a manner ensuring that the temperature does not exceed 80° C. The mixture is then cooled to 20°-50° C., and 69.5 g (1.0 mol) of hydroxylamine hydrochloride is added. There is subsequently added during one hour, while cooling with a water bath, about 92 g (2.3 mols) of solid sodium hydroxide until the pH value of the aqueous solution is 10-11. The organic phase which precipitates is separated, and washed free from salt with water. Distillation yields 245 g (0.92 mol) of 2,2-dimethyl-11-isopropyl-11-amino-undeca-4,8-dienal-oxime; b.p. 158°-162° C./4 Pa; nD20 =1.4930.

후처리

  1. customdoes not exceed 80° C
  2. temperatureThe mixture is then cooled to 20°-50° C.
  3. additionThere is subsequently added during one hour
  4. temperaturewhile cooling with a water bath
  5. customThe organic phase which precipitates
  6. customis separated
  7. washwashed free from salt with water
  8. distillationDistillation

출처 및 근거

ORD 기록
ord-89e944e6f5174d99a2d560e6b6f822f6
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04258176

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