Hydrochloric Acid → 1-(Benzyloxyamino-methyl)-4,4-dimethyl-cyclohexanecarboxylic acid

HRID 2055184노트

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HRID 2055184 반응식
[CH2:1]([O:8][N:9]=[CH:10][C:11]1([C:19]([OH:21])=[O:20])[CH2:16][CH2:15][C:14]([CH3:18])([CH3:17])[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C1C=CC(N=NC2C=CC(S(O)(=O)=O)=CC=2)=CC=1)C.Cl.C([BH3-])#N.[Na+]>CO>[CH2:1]([O:8][NH:9][CH2:10][C:11]1([C:19]([OH:21])=[O:20])[CH2:16][CH2:15][C:14]([CH3:18])([CH3:17])[CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 11037Benzenesulfonic acid, 4-(2-(4-(dimethylamino)phenyl)diazenyl)-HCID 5003444Sodium cyanoborohydrideHCID 866064751-(Benzyloxyimino-methyl)-4,4-dimethyl-cyclohexanecarboxylic acid

생성물 1

HCID 866064761-(Benzyloxyamino-methyl)-4,4-dimethyl-cyclohexanecarboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

A solution of 1-(benzyloxyimino-methyl)-4,4-dimethyl-cyclohexanecarboxylic acid (1.47 g, 5.11 mmol) in methanol (100 mL) at 0° C. under a nitrogen atmosphere was added a trace amount of methyl orange. A solution of saturated methanolic HCl was added until a persistent red color was observed. Sodium cyanoborohydride (0.42 g, 6.68 mmol) was added portionwise alternately with methanolic HCl to maintain the red color. The reaction mixture was maintained at 0° C. for an additional 2 h and the volatiles were removed in vacuo. The product was used without further purification. MH+292.

후처리

  1. temperatureto maintain the red color
  2. customthe volatiles were removed in vacuo
  3. customThe product was used without further purification

출처 및 근거

ORD 기록
ord-5b59443f58024a9cb66f3c3b4fd76fd1
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07332485B2

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