Ammonia → 2-Hydroxymethyl-2-n-propylpropan-1,3-dithiol

HRID 1197337노트

반응식

HRID 1197337 반응식
C([S:8][CH2:9][C:10]([CH2:16][S:17]CC1C=CC=CC=1)([CH2:13][CH2:14][CH3:15])[CH2:11][OH:12])C1C=CC=CC=1.N.[Na].[Cl-].[NH4+]>C(OCC)C.CO>[OH:12][CH2:11][C:10]([CH2:13][CH2:14][CH3:15])([CH2:16][SH:17])[CH2:9][SH:8]

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 193733282,2-Di(benzylthiomethyl)pentan-1-ol

생성물 1

HCID 193733022-Hydroxymethyl-2-n-propylpropan-1,3-dithiol

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매

실험 절차

2,2-Di-(benzylthiomethyl)pentan-1-ol (8.0 g.) in dry diethyl ether (150 ml) was added to liquid ammonia (500 ml) which was stirred under nitrogen at -70°. Sodium (8.0 g.) was added in small pieces and the mixture was stirred at -70° for 3 hours. The mixture was allowed to warm to 20° and solid ammonium chloride (20 g.) was added. This was followed by careful addition of methanol (100 ml) to destroy excess sodium. Water (200 ml) was added and the aqueous mixture was extracted with diethyl ether. The ethereal extracts were dried over anhydrous magnesium sulphate and evaporated in vacuo. 2-Hydroxymethyl-2-n-propylpropan-1,3-dithiol was obtained as a colourless oil (4.6 g.).

후처리

  1. stirringthe mixture was stirred at -70° for 3 hours
  2. temperatureto warm to 20°
  3. customto destroy excess sodium
  4. additionWater (200 ml) was added
  5. extractionthe aqueous mixture was extracted with diethyl ether
  6. dry with materialThe ethereal extracts were dried over anhydrous magnesium sulphate
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-c1588920f9264dff8d39654ad08b99ad
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05116862

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