Sulfuric Acid → HCID 12822286, 화합물

HRID 1112272

반응식

HRID 1112272 반응식
[CH:1]1([N:7]2[CH2:10][CH:9]([C:11]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:12]#N)[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(=O)(=O)(O)[OH:27].[OH-:31].[Na+]>>[CH:1]1([NH:7][CH2:8][CH:9]2[CH2:10][O:31][C:12](=[O:27])[C:11]2([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 12822284alpha-(1-Cyclohexyl-3-azetidinyl)-alpha,alpha-diphenylacetonitrile

생성물 1

HCID 12822286HCID 12822286, 화합물수율 20%

반응 조건

온도
120 °C

실험 절차

To 41.0 g. (0.12 mole) of α-(1-cyclohexyl-3-azetidinyl)-α,α-diphenylacetonitrile was added 100 g. of a 70% solution of sulfuric acid, and the mixture was stirred and heated at 120° C. for 48 hrs. The solution was then poured over ice and made basic with 50% sodium hydroxide, and extracted with chloroform. The organic layer was dried, filtered, and concentrated in vacuo. The residue was crystallized twice from isopropyl ether, the crystallized material weighed 8.0 g. (20% yield) and melted at 129°-131° C.

후처리

  1. additionThe solution was then poured over ice
  2. extractionextracted with chloroform
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was crystallized twice from isopropyl ether

출처 및 근거

ORD 기록
ord-463d7acc1411475190c4a91d36f66e18
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04120969

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