Sulfuric Acid → HCID 178443360, 화합물

HRID 345202노트

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HRID 345202 반응식
[CH2:1]([SH:9])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[OH-].[Na+].[C:12](O)(=O)[CH:13]=[CH2:14].S(=O)(=O)(O)[OH:18]>O.C(O)(C)C>[CH2:4]([CH2:3][CH2:2][C:1]([OH:18])=[S:9])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:12][CH2:13][CH3:14]

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 6581Acrylic AcidHCID 81441-OctanethiolHCID 14798Sodium Hydroxide

생성물 1

HCID 178443360HCID 178443360, 화합물수율 98.6%

시약·촉매·용매 2

HCID 962Water용매2회HCID 3776Isopropanol용매

반응 조건

온도
85 °C

실험 절차

A charge of 146.3 grams (1.00 mole) of n-octylmercaptan, 200 ml. of isopropyl alcohol and 200 ml. of water were added to a round bottom flask. At room temperature, 46.4 grams (1.16 mole) of sodium hydroxide in 46.4 ml. of water were added to the flask, and exotherm proceeded at 50° to 60° C. Over a 30-minute period, 75.1 grams (1.05 mole) of acrylic acid were added dropwise, and the temperature was then raised to 85° C. and the mixture was allowed to reflux for 2 hours. After cooling to 55° C., 83 grams of 70% aqueous sulfuric acid (0.59 mole) were added, with stirring for 30 minutes, followed by pouring into a separatory funnel. The aqueous layer was drained off and the organic layer was washed with an equal volume of water containing 2% sodium sulfate. After vacuum stripping at 60° C., the reaction product was analyzed to contain 0.04 % octylmercaptan and a yield of 98.6% of 3-octylthiopropionic acid product.

후처리

  1. customAt room temperature
  2. customexotherm proceeded at 50° to 60° C
  3. temperatureto reflux for 2 hours
  4. temperatureAfter cooling to 55° C.
  5. additionby pouring into a separatory funnel
  6. washthe organic layer was washed with an equal volume of water containing 2% sodium sulfate
  7. customat 60° C.

출처 및 근거

ORD 기록
ord-96676ddd2c0f46c587043f6b86bca42f
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055606

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